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#$Date: 2021-08-30 14:08:38 +0300 (Mon, 30 Aug 2021) $
#$Revision: 268294 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/44/1564448.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_1564448
loop_
_publ_author_name
'García-Valdivia, Antonio A.'
'Zabala-Lekuona, Andoni'
'Goñi-Cárdenas, Ainhoa'
'Fernández, Belén'
'García, Jose A.'
'Quílez del Moral, José F.'
'Cepeda, Javier'
'Rodríguez-Diéguez, Antonio'
_publ_section_title
;
 Dilution effect on the slow relaxation of a luminescent dysprosium
 Metal-Organic Framework based on 2,5-dihydroxyterephthalic acid
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119687
_journal_paper_doi               10.1016/j.ica.2020.119687
_journal_volume                  509
_journal_year                    2020
_chemical_formula_sum            'C21 H24 Dy N3 O12'
_chemical_formula_weight         672.93
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                104.644(4)
_cell_angle_beta                 107.329(4)
_cell_angle_gamma                97.583(4)
_cell_formula_units_Z            2
_cell_length_a                   10.446(2)
_cell_length_b                   10.877(2)
_cell_length_c                   12.503(3)
_cell_measurement_reflns_used    29920
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.72
_cell_measurement_theta_min      2.94
_cell_volume                     1278.6(5)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker ApexII'
_computing_data_reduction        'Bruker Apex II'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'Phi and Omega Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            34478
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.731
_diffrn_reflns_theta_min         2.228
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.988
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.656
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.0706 before and 0.0469 after correction.
The Ratio of minimum to maximum transmission is 0.9433.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             666
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.077
_refine_diff_density_min         -2.160
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         6582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0297P)²+2.9339P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0624
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6086
_reflns_number_total             6582
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ICA-2020-509-119687.cif
_cod_data_source_block           Compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Empirical' was
changed to 'empirical' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_original_cell_volume        1278.6(4)
_cod_database_code               1564448
_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.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Dy1 Dy 0.09420(2) 0.04651(2) 0.18260(2) 0.00668(4) Uani 1 1 d . . . . .
C1 C 0.2861(3) 0.2721(2) 0.3505(2) 0.0110(5) Uani 1 1 d . . . . .
C2 C 0.3954(3) 0.3907(2) 0.4278(2) 0.0104(5) Uani 1 1 d . . . . .
C3 C 0.5316(3) 0.3923(3) 0.4339(2) 0.0122(5) Uani 1 1 d . . . . .
H3 H 0.5520 0.3200 0.3896 0.015 Uiso 1 1 calc R U . . .
C4 C 0.6368(3) 0.5005(3) 0.5054(2) 0.0119(5) Uani 1 1 d . . . . .
C5 C 0.2056(3) -0.0372(2) -0.0628(2) 0.0104(5) Uani 1 1 d . . . . .
C6 C 0.3572(3) -0.0183(3) -0.0319(2) 0.0103(5) Uani 1 1 d . . . . .
C7 C 0.4414(3) 0.0359(3) 0.0858(2) 0.0141(5) Uani 1 1 d . . . . .
H7 H 0.4015 0.0608 0.1429 0.017 Uiso 1 1 calc R U . . .
C8 C 0.5834(3) 0.0536(3) 0.1197(2) 0.0130(5) Uani 1 1 d . . . . .
C9 C -0.0501(3) -0.2466(2) -0.0092(2) 0.0092(5) Uani 1 1 d . . . . .
C10 C -0.0268(3) -0.3791(2) -0.0071(2) 0.0099(5) Uani 1 1 d . . . . .
C11 C -0.0050(3) -0.4092(3) 0.0977(2) 0.0127(5) Uani 1 1 d . . . . .
H11 H -0.0085 -0.3480 0.1632 0.015 Uiso 1 1 calc R U . . .
C12 C 0.0221(3) -0.5289(3) 0.1071(2) 0.0123(5) Uani 1 1 d . . . . .
C13 C 0.3668(3) -0.0768(3) 0.2946(3) 0.0178(6) Uani 1 1 d . . . . .
H13 H 0.4215 0.0066 0.3182 0.021 Uiso 1 1 calc R U . . .
C14 C 0.3485(4) -0.3008(3) 0.2961(4) 0.0331(8) Uani 1 1 d . . . . .
H14A H 0.3281 -0.3166 0.3621 0.050 Uiso 1 1 calc R U . . .
H14B H 0.4023 -0.3599 0.2714 0.050 Uiso 1 1 calc R U . . .
H14C H 0.2641 -0.3143 0.2324 0.050 Uiso 1 1 calc R U . . .
C15 C 0.5710(4) -0.1359(4) 0.4019(4) 0.0351(9) Uani 1 1 d . . . . .
H15A H 0.6084 -0.0450 0.4181 0.053 Uiso 1 1 calc R U . . .
H15B H 0.6193 -0.1871 0.3600 0.053 Uiso 1 1 calc R U . . .
H15C H 0.5812 -0.1546 0.4746 0.053 Uiso 1 1 calc R U . . .
C16 C -0.0325(3) -0.1112(3) 0.3279(3) 0.0155(5) Uani 1 1 d . . . . .
H16 H -0.1168 -0.1285 0.2680 0.019 Uiso 1 1 calc R U . . .
C17 C 0.1117(4) -0.1724(4) 0.4885(4) 0.0379(10) Uani 1 1 d . . . . .
H17A H 0.1782 -0.1007 0.4912 0.057 Uiso 1 1 calc R U . . .
H17B H 0.1466 -0.2502 0.4764 0.057 Uiso 1 1 calc R U . . .
H17C H 0.0943 -0.1541 0.5615 0.057 Uiso 1 1 calc R U . . .
C18 C -0.1246(4) -0.3017(3) 0.3711(4) 0.0294(8) Uani 1 1 d . . . . .
H18A H -0.2034 -0.3047 0.3060 0.044 Uiso 1 1 calc R U . . .
H18B H -0.1495 -0.2927 0.4402 0.044 Uiso 1 1 calc R U . . .
H18C H -0.0930 -0.3808 0.3532 0.044 Uiso 1 1 calc R U . . .
C19 C 0.5647(18) -0.3047(7) 0.0522(8) 0.234(10) Uani 1 1 d . . . . .
H19 H 0.6443 -0.2821 0.0360 0.281 Uiso 1 1 calc R U . . .
C20 C 0.3429(8) -0.3664(8) -0.0558(18) 0.266(12) Uani 1 1 d . . . . .
H20A H 0.3150 -0.4476 -0.0431 0.399 Uiso 1 1 calc R U . . .
H20B H 0.2884 -0.3687 -0.1334 0.399 Uiso 1 1 calc R U . . .
H20C H 0.3300 -0.2963 0.0015 0.399 Uiso 1 1 calc R U . . .
C21 C 0.508(2) -0.3789(8) -0.1440(13) 0.266(12) Uani 1 1 d . . . . .
H21A H 0.6057 -0.3645 -0.1241 0.399 Uiso 1 1 calc R U . . .
H21B H 0.4726 -0.3257 -0.1915 0.399 Uiso 1 1 calc R U . . .
H21C H 0.4664 -0.4691 -0.1872 0.399 Uiso 1 1 calc R U . . .
N1 N 0.4251(3) -0.1681(3) 0.3299(2) 0.0209(5) Uani 1 1 d . . . . .
N2 N -0.0154(3) -0.1909(3) 0.3922(2) 0.0188(5) Uani 1 1 d . . . . .
N3 N 0.4773(4) -0.3475(3) -0.0453(3) 0.0320(7) Uani 1 1 d . . . . .
O1 O 0.3183(2) 0.17970(19) 0.28658(19) 0.0153(4) Uani 1 1 d . . . . .
O2 O 0.1628(2) 0.2646(2) 0.34915(18) 0.0145(4) Uani 1 1 d . . . . .
O3 O 0.7668(2) 0.4924(2) 0.5084(2) 0.0227(5) Uani 1 1 d . . . . .
O4 O -0.0371(2) -0.16478(17) 0.08689(17) 0.0105(4) Uani 1 1 d . . . . .
O5 O -0.0815(2) -0.22620(18) -0.10867(17) 0.0116(4) Uani 1 1 d . . . . .
O6 O 0.0415(3) -0.5503(2) 0.21286(19) 0.0231(5) Uani 1 1 d . . . . .
O7 O 0.0564(2) -0.0141(2) 0.34153(18) 0.0165(4) Uani 1 1 d . . . . .
O8 O 0.1544(2) -0.01379(19) 0.01785(18) 0.0124(4) Uani 1 1 d . . . . .
O9 O 0.1301(2) -0.07605(19) -0.17161(18) 0.0131(4) Uani 1 1 d . . . . .
O10 O 0.6595(2) 0.1066(3) 0.23691(19) 0.0256(5) Uani 1 1 d . . . . .
O11 O 0.6028(4) -0.2777(4) 0.1493(3) 0.0587(10) Uani 1 1 d . . . . .
O12 O 0.2452(2) -0.0954(2) 0.2328(2) 0.0199(4) 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'
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
O8 Dy1 O4 77.33(7) . .
O8 Dy1 O7 146.28(7) . .
O4 Dy1 O7 78.82(7) . .
O8 Dy1 O5 75.92(7) . 2
O4 Dy1 O5 126.39(7) . 2
O7 Dy1 O5 137.79(7) . 2
O8 Dy1 O1 89.05(7) . .
O4 Dy1 O1 146.07(7) . .
O7 Dy1 O1 97.80(8) . .
O5 Dy1 O1 78.34(7) 2 .
O8 Dy1 O9 122.13(7) . 2
O4 Dy1 O9 78.36(7) . 2
O7 Dy1 O9 75.16(7) . 2
O5 Dy1 O9 78.00(7) 2 2
O1 Dy1 O9 133.92(7) . 2
O8 Dy1 O12 78.22(8) . .
O4 Dy1 O12 73.94(7) . .
O7 Dy1 O12 72.48(8) . .
O5 Dy1 O12 141.30(8) 2 .
O1 Dy1 O12 72.91(7) . .
O9 Dy1 O12 140.64(8) 2 .
O8 Dy1 O2 131.25(7) . .
O4 Dy1 O2 151.22(7) . .
O7 Dy1 O2 76.22(7) . .
O5 Dy1 O2 68.06(7) 2 .
O1 Dy1 O2 52.93(7) . .
O9 Dy1 O2 81.57(7) 2 .
O12 Dy1 O2 111.24(7) . .
O8 Dy1 C1 110.15(8) . .
O4 Dy1 C1 163.53(7) . .
O7 Dy1 C1 87.92(8) . .
O5 Dy1 C1 70.09(7) 2 .
O1 Dy1 C1 26.28(8) . .
O9 Dy1 C1 107.83(8) 2 .
O12 Dy1 C1 92.86(8) . .
O2 Dy1 C1 26.71(7) . .
O8 Dy1 C5 98.50(7) . 2
O4 Dy1 C5 67.14(7) . 2
O7 Dy1 C5 93.78(8) . 2
O5 Dy1 C5 72.04(7) 2 2
O1 Dy1 C5 146.46(7) . 2
O9 Dy1 C5 23.81(7) 2 2
O12 Dy1 C5 140.60(7) . 2
O2 Dy1 C5 100.36(7) . 2
C1 Dy1 C5 124.09(7) . 2
O1 C1 O2 121.0(2) . .
O1 C1 C2 118.7(2) . .
O2 C1 C2 120.3(2) . .
O1 C1 Dy1 55.84(14) . .
O2 C1 Dy1 65.31(14) . .
C2 C1 Dy1 172.90(19) . .
C3 C2 C4 120.1(2) . 2_666
C3 C2 C1 119.0(2) . .
C4 C2 C1 120.9(2) 2_666 .
C4 C3 C2 120.9(2) . .
O3 C4 C3 117.0(2) . .
O3 C4 C2 124.0(2) . 2_666
C3 C4 C2 119.0(2) . 2_666
O8 C5 O9 121.6(2) . .
O8 C5 C6 119.9(2) . .
O9 C5 C6 118.6(2) . .
O8 C5 Dy1 73.83(15) . 2
O9 C5 Dy1 48.62(13) . 2
C6 C5 Dy1 163.45(19) . 2
C7 C6 C8 119.9(2) . 2_655
C7 C6 C5 119.1(2) . .
C8 C6 C5 121.1(2) 2_655 .
C8 C7 C6 121.4(3) . .
O10 C8 C7 118.3(3) . .
O10 C8 C6 123.0(2) . 2_655
C7 C8 C6 118.7(2) . 2_655
O4 C9 O5 125.4(2) . .
O4 C9 C10 117.7(2) . .
O5 C9 C10 116.9(2) . .
C11 C10 C12 119.7(2) . 2_545
C11 C10 C9 118.7(2) . .
C12 C10 C9 121.6(2) 2_545 .
C10 C11 C12 121.7(2) . .
O6 C12 C11 117.7(2) . .
O6 C12 C10 123.7(2) . 2_545
C11 C12 C10 118.6(2) . 2_545
O12 C13 N1 124.5(3) . .
O7 C16 N2 124.8(3) . .
O11 C19 N3 154.7(19) . .
C13 N1 C14 121.6(3) . .
C13 N1 C15 120.0(3) . .
C14 N1 C15 118.5(3) . .
C16 N2 C17 122.1(3) . .
C16 N2 C18 121.5(3) . .
C17 N2 C18 116.4(3) . .
C19 N3 C21 122.9(13) . .
C19 N3 C20 119.2(13) . .
C21 N3 C20 117.9(12) . .
C1 O1 Dy1 97.88(17) . .
C1 O2 Dy1 87.98(16) . .
C9 O4 Dy1 132.11(17) . .
C9 O5 Dy1 138.10(16) . 2
C16 O7 Dy1 123.22(19) . .
C5 O8 Dy1 171.33(19) . .
C5 O9 Dy1 107.57(17) . 2
C13 O12 Dy1 134.0(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O8 2.295(2) .
Dy1 O4 2.3225(19) .
Dy1 O7 2.366(2) .
Dy1 O5 2.3666(19) 2
Dy1 O1 2.368(2) .
Dy1 O9 2.375(2) 2
Dy1 O12 2.410(2) .
Dy1 O2 2.577(2) .
Dy1 C1 2.835(3) .
Dy1 C5 3.018(3) 2
C1 O1 1.267(3) .
C1 O2 1.275(3) .
C1 C2 1.492(3) .
C2 C3 1.399(4) .
C2 C4 1.409(4) 2_666
C3 C4 1.391(4) .
C4 O3 1.362(3) .
C4 C2 1.409(4) 2_666
C5 O8 1.263(3) .
C5 O9 1.278(3) .
C5 C6 1.486(4) .
C5 Dy1 3.018(3) 2
C6 C7 1.393(4) .
C6 C8 1.412(4) 2_655
C7 C8 1.388(4) .
C8 O10 1.367(3) .
C8 C6 1.412(4) 2_655
C9 O4 1.258(3) .
C9 O5 1.272(3) .
C9 C10 1.498(3) .
C10 C11 1.392(4) .
C10 C12 1.409(4) 2_545
C11 C12 1.393(4) .
C12 O6 1.362(3) .
C12 C10 1.409(4) 2_545
C13 O12 1.233(4) .
C13 N1 1.332(4) .
C14 N1 1.445(5) .
C15 N1 1.462(4) .
C16 O7 1.250(4) .
C16 N2 1.319(4) .
C17 N2 1.452(4) .
C18 N2 1.456(4) .
C19 O11 1.104(9) .
C19 N3 1.215(8) .
C20 N3 1.353(9) .
C21 N3 1.337(9) .
O5 Dy1 2.3666(19) 2
O9 Dy1 2.375(2) 2
