#------------------------------------------------------------------------------
#$Date: 2023-12-12 12:07:27 +0200 (Tue, 12 Dec 2023) $
#$Revision: 288244 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/00/1540018.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_1540018
loop_
_publ_author_name
'Liu, Ke'
'Li, Huanhuan'
'Zhang, Xuejing'
'Shi, Wei'
'Cheng, Peng'
_publ_section_title
;
 Constraining and Tuning the Coordination Geometry of a Lanthanide Ion in
 Metal-Organic Frameworks: Approach toward a Single-Molecule Magnet.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10224
_journal_page_last               10231
_journal_paper_doi               10.1021/acs.inorgchem.5b01356
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C24 H20 Dy2 N2 O17'
_chemical_formula_sum            'C24 H20 Dy2 N2 O17'
_chemical_formula_weight         933.42
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.068(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.3085(13)
_cell_length_b                   9.0788(8)
_cell_length_c                   19.6464(19)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9640
_cell_measurement_theta_min      2.4183
_cell_volume                     3240.8(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_sigmaI/netI    0.0840
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5679
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    4.651
_exptl_absorpt_correction_T_max  0.410
_exptl_absorpt_correction_T_min  0.394
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.913
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flaky
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         1.414
_refine_diff_density_min         -1.665
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         2852
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0294P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0920
_reflns_number_gt                2194
_reflns_number_total             2852
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01356_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1540018--1540020.cif.'
_cod_database_code               1540018
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
 C1 \\sim O1: within 1.7A with sigma of 0.005 and sigma for
terminal atoms of 0.01
 O3 \\sim C5: within 1.7A with sigma of 0.005 and sigma for
terminal atoms of 0.01
 C6 \\sim O5: within 1.7A with sigma of 0.005 and sigma for
terminal atoms of 0.01
 C10 \\sim O7: within 1.7A with sigma of 0.005 and sigma for
terminal atoms of 0.01
 C11 \\sim N1: within 1.7A with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C11) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Rotating group:
C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C10(H10)
;
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
O5 O 0.09341(9) 0.5939(2) 0.96614(10) 0.0191(5) Uani 1 1 d U
O2 O 0.36748(10) 0.5537(2) 0.99047(10) 0.0236(6) Uani 1 1 d U
O1 O 0.40657(10) 0.3299(2) 0.95942(10) 0.0241(6) Uani 1 1 d U
C1 C 0.35771(15) 0.4271(4) 0.96656(15) 0.0239(7) Uani 1 1 d U
Dy Dy -0.028456(7) 0.212243(17) 0.997797(7) 0.01863(4) Uani 1 1 d .
O7 O -0.11104(10) 0.2750(2) 0.89925(11) 0.0275(6) Uani 1 1 d U
O6 O 0.00679(9) 0.0411(2) 0.92520(10) 0.0244(6) Uani 1 1 d .
O3 O 0.22500(9) 0.4697(2) 0.95546(10) 0.0204(5) Uani 1 1 d U
O9 O 0.0000 0.0656(3) 1.2500 0.0241(9) Uani 1 2 d S
O8 O -0.02753(10) 0.1764(2) 1.11941(10) 0.0225(6) Uani 1 1 d .
C4 C 0.17733(15) 0.2644(3) 0.90267(15) 0.0205(9) Uani 1 1 d .
H4 H 0.1439 0.1944 0.8833 0.025 Uiso 1 1 calc R
N1 N -0.22867(13) 0.2890(4) 0.84803(14) 0.0399(3) Uani 1 1 d U
O4 O 0.03425(9) 0.3810(2) 0.93884(9) 0.0187(6) Uani 1 1 d .
C10 C -0.17681(16) 0.3066(4) 0.90028(17) 0.0371(4) Uani 1 1 d U
H10 H -0.1905 0.3453 0.9407 0.044 Uiso 1 1 calc R
C9 C -0.01327(14) 0.0415(3) 1.12590(14) 0.0173(7) Uani 1 1 d U
C3 C 0.25443(16) 0.2558(4) 0.90730(16) 0.0243(9) Uani 1 1 d .
H3 H 0.2819 0.1807 0.8906 0.029 Uiso 1 1 calc R
C7 C -0.00269(15) -0.1671(4) 1.21319(14) 0.0228(9) Uani 1 1 d .
H7 H -0.0045 -0.2495 1.1849 0.027 Uiso 1 1 calc R
C6 C 0.09056(14) 0.4621(3) 0.94686(14) 0.0169(7) Uani 1 1 d U
C8 C -0.00461(14) -0.0251(4) 1.19277(15) 0.0208(9) Uani 1 1 d .
C2 C 0.28106(14) 0.3795(4) 0.94110(14) 0.0206(9) Uani 1 1 d .
C5 C 0.16066(14) 0.3940(4) 0.93176(14) 0.0180(7) Uani 1 1 d U
C12 C -0.30641(15) 0.3285(4) 0.85313(18) 0.0444(12) Uani 1 1 d .
H12A H -0.3364 0.2415 0.8476 0.067 Uiso 1 1 calc R
H12B H -0.3231 0.3981 0.8179 0.067 Uiso 1 1 calc R
H12C H -0.3101 0.3714 0.8972 0.067 Uiso 1 1 calc R
C11 C -0.21403(18) 0.2202(4) 0.78524(18) 0.0458(5) Uani 1 1 d U
H11A H -0.2208 0.2907 0.7486 0.069 Uiso 1 1 calc R
H11B H -0.2473 0.1392 0.7750 0.069 Uiso 1 1 calc R
H11C H -0.1643 0.1847 0.7902 0.069 Uiso 1 1 calc R
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'
Dy Dy -0.1892 4.4098 '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'
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
C6 O5 Dy 145.55(17) . 5_567
C1 O2 Dy 131.14(18) . 3
C1 O1 Dy 136.96(19) . 7_557
O2 C1 O1 127.5(3) . .
O2 C1 C2 118.5(3) . .
O1 C1 C2 113.9(3) . .
O6 Dy O5 157.92(6) . 5_567
O6 Dy O4 86.64(7) . .
O5 Dy O4 87.38(7) 5_567 .
O6 Dy O1 77.18(7) . 7_557
O5 Dy O1 121.96(7) 5_567 7_557
O4 Dy O1 77.03(7) . 7_557
O6 Dy O7 81.53(7) . .
O5 Dy O7 76.38(7) 5_567 .
O4 Dy O7 74.81(7) . .
O1 Dy O7 145.43(7) 7_557 .
O6 Dy O2 80.45(7) . 3_445
O5 Dy O2 92.38(7) 5_567 3_445
O4 Dy O2 144.60(6) . 3_445
O1 Dy O2 130.58(7) 7_557 3_445
O7 Dy O2 70.78(7) . 3_445
O6 Dy O8 124.48(7) . .
O5 Dy O8 74.76(7) 5_567 .
O4 Dy O8 130.07(7) . .
O1 Dy O8 74.28(7) 7_557 .
O7 Dy O8 140.09(7) . .
O2 Dy O8 83.46(7) 3_445 .
O6 Dy O6 74.88(7) . 5_557
O5 Dy O6 121.21(6) 5_567 5_557
O4 Dy O6 141.48(6) . 5_557
O1 Dy O6 66.16(6) 7_557 5_557
O7 Dy O6 133.02(7) . 5_557
O2 Dy O6 65.67(6) 3_445 5_557
O8 Dy O6 50.18(6) . 5_557
O6 Dy C9 100.01(8) . .
O5 Dy C9 97.97(7) 5_567 .
O4 Dy C9 141.13(7) . .
O1 Dy C9 67.48(7) 7_557 .
O7 Dy C9 143.92(7) . .
O2 Dy C9 73.94(7) 3_445 .
O8 Dy C9 24.68(8) . .
O6 Dy C9 25.52(7) 5_557 .
O6 Dy Dy 41.79(5) . 5_557
O5 Dy Dy 151.85(5) 5_567 5_557
O4 Dy Dy 120.46(5) . 5_557
O1 Dy Dy 66.14(5) 7_557 5_557
O7 Dy Dy 112.81(6) . 5_557
O2 Dy Dy 67.78(5) 3_445 5_557
O8 Dy Dy 83.00(5) . 5_557
O6 Dy Dy 33.09(4) 5_557 5_557
C9 Dy Dy 58.36(6) . 5_557
C10 O7 Dy 124.3(2) . .
C9 O6 Dy 165.43(17) 5_557 .
C9 O6 Dy 85.41(17) 5_557 5_557
Dy O6 Dy 105.12(7) . 5_557
C2 O3 C5 105.1(2) . .
C8 O9 C8 107.2(3) . 2_557
C9 O8 Dy 102.04(17) . .
C5 C4 C3 107.3(3) . .
C10 N1 C11 121.9(3) . .
C10 N1 C12 121.5(3) . .
C11 N1 C12 116.4(3) . .
C6 O4 Dy 140.71(17) . .
O7 C10 N1 124.5(3) . .
O8 C9 O6 122.3(3) . 5_557
O8 C9 C8 120.1(3) . .
O6 C9 C8 117.6(3) 5_557 .
O8 C9 Dy 53.28(14) . .
O6 C9 Dy 69.07(16) 5_557 .
C8 C9 Dy 173.1(2) . .
C2 C3 C4 106.3(3) . .
C8 C7 C7 107.18(18) . 2_557
O5 C6 O4 126.7(2) . .
O5 C6 C5 116.9(2) . .
O4 C6 C5 116.4(3) . .
C7 C8 O9 109.2(3) . .
C7 C8 C9 132.1(3) . .
O9 C8 C9 118.6(3) . .
C3 C2 O3 111.1(2) . .
C3 C2 C1 131.7(3) . .
O3 C2 C1 117.1(3) . .
C4 C5 O3 110.1(2) . .
C4 C5 C6 133.5(3) . .
O3 C5 C6 116.3(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O5 C6 1.254(4) .
O5 Dy 2.285(2) 5_567
O2 C1 1.246(4) .
O2 Dy 2.3782(19) 3
O1 C1 1.276(4) .
O1 Dy 2.3176(18) 7_557
C1 C2 1.494(4) .
Dy O6 2.257(2) .
Dy O5 2.285(2) 5_567
Dy O4 2.309(2) .
Dy O1 2.3175(18) 7_557
Dy O7 2.375(2) .
Dy O2 2.3782(19) 3_445
Dy O8 2.409(2) .
Dy O6 2.754(2) 5_557
Dy C9 2.940(3) .
Dy Dy 3.9904(5) 5_557
O7 C10 1.240(4) .
O6 C9 1.270(4) 5_557
O6 Dy 2.754(2) 5_557
O3 C2 1.369(3) .
O3 C5 1.393(3) .
O9 C8 1.388(3) .
O9 C8 1.388(3) 2_557
O8 C9 1.255(4) .
C4 C5 1.359(4) .
C4 C3 1.405(4) .
N1 C10 1.319(4) .
N1 C11 1.437(5) .
N1 C12 1.483(4) .
O4 C6 1.261(3) .
C9 O6 1.270(4) 5_557
C9 C8 1.437(4) .
C3 C2 1.364(4) .
C7 C8 1.349(4) .
C7 C7 1.437(6) 2_557
C6 C5 1.487(4) .
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
_platon_squeeze_void_content
1 0.500 -0.112 0.250 154 53 ' '
2 0.500 0.111 0.750 154 56 ' '
3 0.000 0.388 0.250 154 53 ' '
4 0.000 0.611 0.750 154 56 ' '
