#------------------------------------------------------------------------------
#$Date: 2021-03-29 10:21:57 +0300 (Mon, 29 Mar 2021) $
#$Revision: 263405 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/13/1561322.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_1561322
loop_
_publ_author_name
'Zhang, Xiu-Mei'
'Li, Peng'
'Gao, Wei'
'Liu, Feng'
'Liu, Jie-Ping'
_publ_section_title
;
 Construction of three lanthanide metal-organic frameworks: Synthesis,
 structure, magnetic properties and highly selective sensing of metal ions
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              6
_journal_page_last               11
_journal_paper_doi               10.1016/j.jssc.2016.09.009
_journal_volume                  244
_journal_year                    2016
_chemical_formula_sum            'C9 H17 Dy N4 O11'
_chemical_formula_weight         519.77
_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   mixed
_cell_angle_alpha                111.817(4)
_cell_angle_beta                 99.390(4)
_cell_angle_gamma                100.699(4)
_cell_formula_units_Z            2
_cell_length_a                   7.4832(10)
_cell_length_b                   10.9344(13)
_cell_length_c                   11.4824(15)
_cell_measurement_reflns_used    9222
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      3.06
_cell_volume                     828.86(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13312
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.005
_diffrn_reflns_theta_max         25.005
_diffrn_reflns_theta_min         3.038
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.573
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.083
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             506
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.0194(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         2902
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0135
_refine_ls_R_factor_gt           0.0130
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0126P)²+0.7350P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0321
_refine_ls_wR_factor_ref         0.0323
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2834
_reflns_number_total             2902
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            mmc6.cif
_cod_data_source_block           3
_cod_database_code               1561322
_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   0.462
_shelx_estimated_absorpt_t_max   0.711
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 0.66324(2) 0.75660(2) 0.66476(2) 0.01480(6) Uani 1 1 d . . . . .
C1 C 0.4399(3) 0.5670(2) 0.3422(2) 0.0185(5) Uani 1 1 d . . . . .
C2 C 0.4039(3) 0.6271(2) 0.2445(2) 0.0165(4) Uani 1 1 d . . . . .
C3 C 0.4326(3) 0.7688(2) 0.2874(2) 0.0165(4) Uani 1 1 d . . . . .
H3A H 0.4849 0.8262 0.3747 0.020 Uiso 1 1 calc R U . . .
C4 C 0.3822(3) 0.8232(2) 0.1986(2) 0.0162(4) Uani 1 1 d . . . . .
C5 C 0.3859(3) 0.9718(2) 0.2452(2) 0.0161(4) Uani 1 1 d . . . . .
C6 C 0.3081(3) 0.7371(2) 0.0676(2) 0.0185(5) Uani 1 1 d . . . . .
H6A H 0.2750 0.7739 0.0087 0.022 Uiso 1 1 calc R U . . .
C7 C 0.2827(3) 0.5957(2) 0.0235(2) 0.0175(5) Uani 1 1 d . . . . .
C8 C 0.3308(3) 0.5417(2) 0.1136(2) 0.0187(5) Uani 1 1 d . . . . .
H8A H 0.3136 0.4479 0.0855 0.022 Uiso 1 1 calc R U . . .
C9 C 0.1954(3) 0.5074(2) -0.1146(2) 0.0202(5) Uani 1 1 d . . . . .
O1 O 0.4930(3) 0.64762(18) 0.45987(16) 0.0344(5) Uani 1 1 d . . . . .
O2 O 0.4112(3) 0.43973(16) 0.30007(16) 0.0273(4) Uani 1 1 d . . . . .
O3 O 0.4748(2) 1.05673(15) 0.35782(15) 0.0196(3) Uani 1 1 d . . . . .
O4 O 0.2873(2) 1.00977(16) 0.17002(16) 0.0218(4) Uani 1 1 d . . . . .
O5 O 0.4027(3) 0.7556(2) 0.7515(3) 0.0472(6) Uani 1 1 d D . . . .
H5A H 0.371(5) 0.827(2) 0.787(4) 0.071 Uiso 1 1 d D U . . .
H5B H 0.338(5) 0.689(2) 0.759(4) 0.071 Uiso 1 1 d D U . . .
O6 O 0.8705(3) 0.8963(2) 0.6012(2) 0.0374(5) Uani 1 1 d D . . . .
H6B H 0.834(4) 0.957(3) 0.584(4) 0.056 Uiso 1 1 d D U . . .
H6C H 0.975(3) 0.893(3) 0.587(4) 0.056 Uiso 1 1 d D U . . .
O7 O 0.8760(3) 0.6284(2) 0.5733(2) 0.0422(5) Uani 1 1 d D . . . .
H7A H 0.884(5) 0.606(4) 0.4980(15) 0.063 Uiso 1 1 d D U . . .
H7B H 0.918(5) 0.584(3) 0.609(3) 0.063 Uiso 1 1 d D U . . .
O8 O 0.9184(3) 0.7919(2) 0.83685(18) 0.0302(4) Uani 1 1 d D . . . .
H8B H 0.909(4) 0.797(3) 0.9102(16) 0.045 Uiso 1 1 d D U . . .
H8C H 1.022(3) 0.839(3) 0.842(3) 0.045 Uiso 1 1 d D U . . .
O9 O 0.7043(4) 0.0247(2) 0.0932(2) 0.0556(6) Uani 1 1 d D . . . .
H9B H 0.742(6) -0.037(4) 0.099(5) 0.083 Uiso 1 1 d D U . . .
O10 O 0.0945(3) 0.1611(2) 0.9157(2) 0.0350(4) Uani 1 1 d D . . . .
H10A H -0.012(3) 0.106(3) 0.879(3) 0.052 Uiso 1 1 d D U . . .
H10B H 0.106(4) 0.226(2) 0.894(3) 0.052 Uiso 1 1 d D U . . .
O11 O 0.8284(2) 1.08862(18) 0.50469(18) 0.0290(4) Uani 1 1 d D . . . .
H11A H 0.872(4) 1.1640(18) 0.567(2) 0.043 Uiso 1 1 d D U . . .
H11B H 0.725(3) 1.081(3) 0.460(2) 0.043 Uiso 1 1 d D U . . .
N1 N 0.1138(3) 0.3733(2) -0.16322(19) 0.0258(5) Uani 1 1 d . . . . .
N2 N 0.0450(3) 0.3352(2) -0.2905(2) 0.0335(5) Uani 1 1 d . . . . .
N3 N 0.0861(4) 0.4412(2) -0.3177(2) 0.0414(6) Uani 1 1 d . . . . .
N4 N 0.1825(4) 0.5523(2) -0.2085(2) 0.0380(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'
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'
H H 0.0000 0.0000 '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 O2 91.58(6) . 2_666
O1 Dy1 O5 94.33(9) . .
O2 Dy1 O5 71.06(7) 2_666 .
O1 Dy1 O6 89.11(8) . .
O2 Dy1 O6 148.03(7) 2_666 .
O5 Dy1 O6 140.74(7) . .
O1 Dy1 O8 152.23(7) . .
O2 Dy1 O8 76.52(7) 2_666 .
O5 Dy1 O8 105.00(9) . .
O6 Dy1 O8 88.31(7) . .
O1 Dy1 O7 81.09(8) . .
O2 Dy1 O7 75.97(7) 2_666 .
O5 Dy1 O7 146.59(7) . .
O6 Dy1 O7 72.57(7) . .
O8 Dy1 O7 71.77(7) . .
O1 Dy1 O4 132.16(6) . 2_676
O2 Dy1 O4 124.52(6) 2_666 2_676
O5 Dy1 O4 73.09(7) . 2_676
O6 Dy1 O4 75.80(7) . 2_676
O8 Dy1 O4 73.61(6) . 2_676
O7 Dy1 O4 133.11(8) . 2_676
O1 Dy1 O3 80.10(6) . 2_676
O2 Dy1 O3 141.54(6) 2_666 2_676
O5 Dy1 O3 72.23(6) . 2_676
O6 Dy1 O3 69.90(6) . 2_676
O8 Dy1 O3 124.48(6) . 2_676
O7 Dy1 O3 137.97(6) . 2_676
O4 Dy1 O3 52.06(5) 2_676 2_676
O1 Dy1 C5 105.92(6) . 2_676
O2 Dy1 C5 139.95(6) 2_666 2_676
O5 Dy1 C5 71.90(6) . 2_676
O6 Dy1 C5 69.57(7) . 2_676
O8 Dy1 C5 99.03(7) . 2_676
O7 Dy1 C5 141.28(7) . 2_676
O4 Dy1 C5 26.27(6) 2_676 2_676
O3 Dy1 C5 25.85(6) 2_676 2_676
O1 C1 O2 124.6(2) . .
O1 C1 C2 117.68(19) . .
O2 C1 C2 117.7(2) . .
C8 C2 C3 120.2(2) . .
C8 C2 C1 120.10(19) . .
C3 C2 C1 119.6(2) . .
C4 C3 C2 119.7(2) . .
C4 C3 H3A 120.2 . .
C2 C3 H3A 120.2 . .
C6 C4 C3 120.0(2) . .
C6 C4 C5 119.4(2) . .
C3 C4 C5 120.3(2) . .
O3 C5 O4 119.86(19) . .
O3 C5 C4 121.41(19) . .
O4 C5 C4 118.6(2) . .
O3 C5 Dy1 61.40(11) . 2_676
O4 C5 Dy1 58.66(11) . 2_676
C4 C5 Dy1 171.63(15) . 2_676
C4 C6 C7 120.7(2) . .
C4 C6 H6A 119.6 . .
C7 C6 H6A 119.6 . .
C8 C7 C6 118.9(2) . .
C8 C7 C9 121.8(2) . .
C6 C7 C9 119.1(2) . .
C2 C8 C7 120.5(2) . .
C2 C8 H8A 119.7 . .
C7 C8 H8A 119.7 . .
N1 C9 N4 110.7(2) . .
N1 C9 C7 125.2(2) . .
N4 C9 C7 124.1(2) . .
C1 O1 Dy1 161.03(18) . .
C1 O2 Dy1 148.56(16) . 2_666
C5 O3 Dy1 92.75(13) . 2_676
C5 O4 Dy1 95.07(13) . 2_676
Dy1 O5 H5A 122(2) . .
Dy1 O5 H5B 126(2) . .
H5A O5 H5B 111.3(18) . .
Dy1 O6 H6B 118(2) . .
Dy1 O6 H6C 131(2) . .
H6B O6 H6C 111.3(17) . .
Dy1 O7 H7A 124(2) . .
Dy1 O7 H7B 118(2) . .
H7A O7 H7B 114.7(18) . .
Dy1 O8 H8B 125(2) . .
Dy1 O8 H8C 117(2) . .
H8B O8 H8C 110.7(17) . .
H10A O10 H10B 111.1(17) . .
H11A O11 H11B 113.3(17) . .
C9 N1 N2 105.5(2) . .
N3 N2 N1 109.3(2) . .
N2 N3 N4 109.5(2) . .
C9 N4 N3 105.0(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O1 2.2253(17) .
Dy1 O2 2.3143(16) 2_666
Dy1 O5 2.3301(19) .
Dy1 O6 2.3643(18) .
Dy1 O8 2.3721(18) .
Dy1 O7 2.4257(19) .
Dy1 O4 2.4657(16) 2_676
Dy1 O3 2.5277(15) 2_676
Dy1 C5 2.876(2) 2_676
C1 O1 1.253(3) .
C1 O2 1.254(3) .
C1 C2 1.510(3) .
C2 C8 1.389(3) .
C2 C3 1.401(3) .
C3 C4 1.395(3) .
C3 H3A 0.9300 .
C4 C6 1.392(3) .
C4 C5 1.504(3) .
C5 O3 1.255(3) .
C5 O4 1.278(3) .
C5 Dy1 2.876(2) 2_676
C6 C7 1.401(3) .
C6 H6A 0.9300 .
C7 C8 1.399(3) .
C7 C9 1.471(3) .
C8 H8A 0.9300 .
C9 N1 1.335(3) .
C9 N4 1.338(3) .
O2 Dy1 2.3143(16) 2_666
O3 Dy1 2.5277(15) 2_676
O4 Dy1 2.4657(16) 2_676
O5 H5A 0.831(10) .
O5 H5B 0.832(10) .
O6 H6B 0.832(10) .
O6 H6C 0.831(10) .
O7 H7A 0.823(10) .
O7 H7B 0.817(10) .
O8 H8B 0.838(10) .
O8 H8C 0.830(10) .
O9 H9B 0.797(19) .
O10 H10A 0.837(10) .
O10 H10B 0.831(10) .
O11 H11A 0.828(10) .
O11 H11B 0.825(10) .
N1 N2 1.341(3) .
N2 N3 1.305(3) .
N3 N4 1.347(3) .
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
O5 H5A O9 0.831(10) 1.944(15) 2.754(3) 165(4) 2_666
O5 H5B N4 0.832(10) 1.912(12) 2.741(3) 174(4) 1_556
O6 H6B O11 0.832(10) 1.978(17) 2.759(3) 156(3) .
O6 H6C O11 0.831(10) 1.966(18) 2.736(3) 154(3) 2_776
O7 H7A N3 0.823(10) 2.000(10) 2.822(3) 178(4) 2_665
O7 H7B N3 0.817(10) 2.467(14) 3.268(3) 167(3) 1_656
O8 H8B O10 0.838(10) 1.884(12) 2.714(3) 171(3) 2_667
O8 H8C O9 0.830(10) 2.123(14) 2.933(4) 165(3) 2_766
O9 H9B O10 0.797(19) 1.97(3) 2.728(3) 159(5) 2_656
O10 H10A O4 0.837(10) 2.069(13) 2.891(3) 167(4) 2_566
O10 H10B N1 0.831(10) 1.947(11) 2.776(3) 176(3) 1_556
O11 H11A N2 0.828(10) 1.996(12) 2.802(3) 164(3) 1_666
O11 H11B O3 0.825(10) 1.956(10) 2.780(2) 177(3) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
O1 C1 C2 C8 -175.0(2) . . . .
O2 C1 C2 C8 3.8(3) . . . .
O1 C1 C2 C3 0.7(3) . . . .
O2 C1 C2 C3 179.5(2) . . . .
C8 C2 C3 C4 1.9(3) . . . .
C1 C2 C3 C4 -173.8(2) . . . .
C2 C3 C4 C6 -1.5(3) . . . .
C2 C3 C4 C5 171.2(2) . . . .
C6 C4 C5 O3 -169.7(2) . . . .
C3 C4 C5 O3 17.6(3) . . . .
C6 C4 C5 O4 14.2(3) . . . .
C3 C4 C5 O4 -158.5(2) . . . .
C3 C4 C6 C7 0.1(3) . . . .
C5 C4 C6 C7 -172.6(2) . . . .
C4 C6 C7 C8 0.9(3) . . . .
C4 C6 C7 C9 177.0(2) . . . .
C3 C2 C8 C7 -0.8(4) . . . .
C1 C2 C8 C7 174.8(2) . . . .
C6 C7 C8 C2 -0.5(3) . . . .
C9 C7 C8 C2 -176.6(2) . . . .
C8 C7 C9 N1 16.6(4) . . . .
C6 C7 C9 N1 -159.5(2) . . . .
C8 C7 C9 N4 -165.5(3) . . . .
C6 C7 C9 N4 18.5(4) . . . .
O2 C1 O1 Dy1 55.9(7) . . . .
C2 C1 O1 Dy1 -125.5(4) . . . .
O1 C1 O2 Dy1 25.0(5) . . . 2_666
C2 C1 O2 Dy1 -153.6(2) . . . 2_666
O4 C5 O3 Dy1 5.2(2) . . . 2_676
C4 C5 O3 Dy1 -170.89(18) . . . 2_676
O3 C5 O4 Dy1 -5.3(2) . . . 2_676
C4 C5 O4 Dy1 170.86(17) . . . 2_676
N4 C9 N1 N2 -1.4(3) . . . .
C7 C9 N1 N2 176.8(2) . . . .
C9 N1 N2 N3 1.0(3) . . . .
N1 N2 N3 N4 -0.3(3) . . . .
N1 C9 N4 N3 1.2(3) . . . .
C7 C9 N4 N3 -177.1(2) . . . .
N2 N3 N4 C9 -0.5(3) . . . .
