#------------------------------------------------------------------------------
#$Date: 2021-04-12 10:54:55 +0200 (lun 12 de abr de 2021) $
#$Revision: 264052 $
#$URL: svn://www.crystallography.net/cod/cif/1/56/16/1561657.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_1561657
loop_
_publ_author_name
'Igoa, Fernando'
'Peinado, Guzmán'
'Suescun, Leopoldo'
'Kremer, Carlos'
'Torres, Julia'
_publ_section_title
;
 Design of a white-light emitting material based on a mixed-lanthanide
 metal organic framework
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              120925
_journal_paper_doi               10.1016/j.jssc.2019.120925
_journal_volume                  279
_journal_year                    2019
_chemical_formula_sum            'C24 H36 Dy1.6 Eu0.38 O39 Tb0.02 Zn3'
_chemical_formula_weight         1465.56
_space_group_crystal_system      hexagonal
_space_group_IT_number           192
_space_group_name_Hall           '-P 6 2c'
_space_group_name_H-M_alt        'P 6/m c c'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.632(4)
_cell_length_b                   14.632(4)
_cell_length_c                   15.737(3)
_cell_measurement_reflns_used    15036
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.22
_cell_measurement_theta_min      3.794
_cell_volume                     2917.8(13)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 10.83333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       'ω and \j scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0094
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            65834
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.344
_diffrn_reflns_theta_min         3.047
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.755
_exptl_absorpt_correction_T_max  0.0962
_exptl_absorpt_correction_T_min  0.0632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_description       'hexagonal needle'
_exptl_crystal_F_000             1426
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.137
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         930
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0325
_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)+(0.0724P)²+9.0706P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1239
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                745
_reflns_number_total             930
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            JSSC-2019-279-120925.cif
_cod_data_source_block           ETD_2_02_
_cod_original_cell_volume        2917.7(16)
_cod_original_formula_sum        'C24 H36 Dy1.60 Eu0.38 O39 Tb0.02 Zn3'
_cod_database_code               1561657
_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   0.547
_shelx_estimated_absorpt_t_max   0.834
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-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'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'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'
'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_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 0.6667 0.3333 0.2500 0.0286(3) Uani 0.8 6 d S T P A .
Eu1 Eu 0.6667 0.3333 0.2500 0.0286(3) Uani 0.19 6 d S T P A .
Tb1 Tb 0.6667 0.3333 0.2500 0.0286(3) Uani 0.01 6 d S T P A .
Zn1 Zn 0.5000 0.0000 0.5000 0.0281(3) Uani 1 4 d S T P . .
O1 O 0.5793(3) 0.1944(3) 0.3547(3) 0.0394(9) Uani 1 1 d . . . . .
C1 C 0.4811(5) 0.1311(5) 0.3608(4) 0.0409(13) Uani 1 1 d . . . . .
C2 C 0.4055(12) 0.1566(13) 0.3118(11) 0.040(3) Uani 0.62(3) 1 d . . P A 1
H2A H 0.3504 0.0937 0.2843 0.047 Uiso 0.62(3) 1 calc R U P A 1
H2B H 0.3728 0.1839 0.3501 0.047 Uiso 0.62(3) 1 calc R U P A 1
C2A C 0.420(2) 0.137(2) 0.2856(19) 0.040(3) Uani 0.38(3) 1 d . . P A 2
H2C H 0.4126 0.0853 0.2434 0.047 Uiso 0.38(3) 1 calc R U P A 2
H2D H 0.3497 0.1193 0.3040 0.047 Uiso 0.38(3) 1 calc R U P A 2
O2 O 0.4379(3) 0.0547(3) 0.4093(3) 0.0565(13) Uani 1 1 d . . . . .
O3 O 0.4684(4) 0.2342(2) 0.2500 0.0366(12) Uani 1 2 d S T P . .
O1W O 0.6509(4) 0.1443(4) 0.5000 0.0378(12) Uani 1 2 d DS T P . .
H1W H 0.639(5) 0.170(4) 0.4577(3) 0.050(19) Uiso 1 1 d D . . . .
O2W O 0.212(3) -0.018(3) 0.532(2) 0.180(17) Uiso 0.25 1 d . . P . .
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'
Eu Eu -0.1578 3.6682 '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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 '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 Dy1 O1 78.95(15) . 2_655
O1 Dy1 O1 86.9(2) . 11_655
O1 Dy1 O1 125.67(17) 2_655 11_655
O1 Dy1 O1 148.73(18) . 10_665
O1 Dy1 O1 86.9(2) 2_655 10_665
O1 Dy1 O1 78.95(15) 11_655 10_665
O1 Dy1 O1 125.67(17) . 12
O1 Dy1 O1 148.73(18) 2_655 12
O1 Dy1 O1 78.95(15) 11_655 12
O1 Dy1 O1 78.95(15) 10_665 12
O1 Dy1 O1 78.95(15) . 3_665
O1 Dy1 O1 78.95(15) 2_655 3_665
O1 Dy1 O1 148.73(18) 11_655 3_665
O1 Dy1 O1 125.67(17) 10_665 3_665
O1 Dy1 O1 86.9(2) 12 3_665
O1 Dy1 O3 62.83(9) . .
O1 Dy1 O3 136.56(10) 2_655 .
O1 Dy1 O3 74.36(9) 11_655 .
O1 Dy1 O3 136.56(10) 10_665 .
O1 Dy1 O3 62.83(9) 12 .
O1 Dy1 O3 74.36(9) 3_665 .
O1 Dy1 O3 74.36(9) . 2_655
O1 Dy1 O3 62.83(9) 2_655 2_655
O1 Dy1 O3 62.83(9) 11_655 2_655
O1 Dy1 O3 74.36(9) 10_665 2_655
O1 Dy1 O3 136.56(10) 12 2_655
O1 Dy1 O3 136.56(10) 3_665 2_655
O3 Dy1 O3 120.0 . 2_655
O1 Dy1 O3 136.56(10) . 3_665
O1 Dy1 O3 74.36(9) 2_655 3_665
O1 Dy1 O3 136.56(10) 11_655 3_665
O1 Dy1 O3 62.83(9) 10_665 3_665
O1 Dy1 O3 74.36(9) 12 3_665
O1 Dy1 O3 62.83(9) 3_665 3_665
O3 Dy1 O3 120.0 . 3_665
O3 Dy1 O3 120.000(1) 2_655 3_665
O2 Zn1 O2 92.1(3) 13_656 16_556
O2 Zn1 O2 87.9(3) 13_656 4_655
O2 Zn1 O2 180.00(18) 16_556 4_655
O2 Zn1 O2 180.00(18) 13_656 .
O2 Zn1 O2 87.9(3) 16_556 .
O2 Zn1 O2 92.1(3) 4_655 .
O2 Zn1 O1W 93.11(16) 13_656 13_656
O2 Zn1 O1W 86.89(16) 16_556 13_656
O2 Zn1 O1W 93.11(16) 4_655 13_656
O2 Zn1 O1W 86.89(16) . 13_656
O2 Zn1 O1W 86.89(16) 13_656 .
O2 Zn1 O1W 93.11(16) 16_556 .
O2 Zn1 O1W 86.89(16) 4_655 .
O2 Zn1 O1W 93.11(16) . .
O1W Zn1 O1W 180.0 13_656 .
C1 O1 Dy1 126.5(4) . .
O2 C1 O1 126.1(5) . .
O2 C1 C2A 119.0(12) . .
O1 C1 C2A 112.8(11) . .
O2 C1 C2 115.1(7) . .
O1 C1 C2 118.4(7) . .
O3 C2 C1 106.1(10) . .
O3 C2 H2A 110.5 . .
C1 C2 H2A 110.5 . .
O3 C2 H2B 110.5 . .
C1 C2 H2B 110.5 . .
H2A C2 H2B 108.7 . .
O3 C2A C1 112(2) . .
O3 C2A H2C 109.3 . .
C1 C2A H2C 109.3 . .
O3 C2A H2D 109.3 . .
C1 C2A H2D 109.3 . .
H2C C2A H2D 108.0 . .
C1 O2 Zn1 131.0(4) . .
C2A O3 C2A 126(2) . 12
C2 O3 C2 112.1(12) . 12
C2A O3 Dy1 117.0(12) . .
C2A O3 Dy1 117.0(12) 12 .
C2 O3 Dy1 124.0(6) . .
C2 O3 Dy1 124.0(6) 12 .
Zn1 O1W H1W 96(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O1 2.425(4) .
Dy1 O1 2.425(4) 2_655
Dy1 O1 2.425(4) 11_655
Dy1 O1 2.425(4) 10_665
Dy1 O1 2.425(4) 12
Dy1 O1 2.425(4) 3_665
Dy1 O3 2.512(5) .
Dy1 O3 2.512(5) 2_655
Dy1 O3 2.512(5) 3_665
Zn1 O2 2.056(4) 13_656
Zn1 O2 2.056(4) 16_556
Zn1 O2 2.056(4) 4_655
Zn1 O2 2.056(4) .
Zn1 O1W 2.162(5) 13_656
Zn1 O1W 2.162(5) .
O1 C1 1.264(7) .
C1 O2 1.236(7) .
C1 C2A 1.51(3) .
C1 C2 1.540(15) .
C2 O3 1.427(15) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C2A O3 1.36(3) .
C2A H2C 0.9700 .
C2A H2D 0.9700 .
O3 C2A 1.36(3) 12
O3 C2 1.427(15) 12
O1W H1W 0.832(10) .
O2W O2W 1.01(7) 16_556
