#------------------------------------------------------------------------------
#$Date: 2019-11-17 10:11:44 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229278 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/77/7047748.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_7047748
loop_
_publ_author_name
'Yang, Chun'
'Zheng, Jie-Yu'
'Cai, Wen-Jing'
'Guo, Fu-Sheng'
'Wang, Yao-Yu'
_publ_section_title
;
 Two isostructural Ln-MOFs showing luminescent sensing (Eu) and slow
 magnetic relaxation (Dy) properties.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15656
_journal_page_last               15660
_journal_paper_doi               10.1039/c8dt03458c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C28 H19 Dy N2 O8 S2, H2 O'
_chemical_formula_sum            'C28 H21 Dy N2 O9 S2'
_chemical_formula_weight         756.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-19 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.934(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1939(16)
_cell_length_b                   12.4831(14)
_cell_length_c                   15.9204(18)
_cell_measurement_reflns_used    3694
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.495
_cell_measurement_theta_min      2.722
_cell_volume                     2651.8(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14028
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.663
_exptl_absorpt_coefficient_mu    3.037
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1025 before and 0.0546 after correction. The Ratio of minimum to maximum transmission is 0.8277. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.894
_exptl_crystal_description       block
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.391
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5175
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0368
_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)+(0.0879P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1421
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4033
_reflns_number_total             5175
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt03458c2.cif
_cod_data_source_block           dy
_cod_depositor_comments
'Adding full bibliography for 7047747--7047748.cif.'
_cod_database_code               7047748
_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_max   0.793
_shelx_estimated_absorpt_t_min   0.712
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3.a Riding coordinates:
 O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C23(H23A,H23B)
3.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3), C5(H5), C8(H8), C11(H11), C12(H12), C13(H13), C14(H14),
 C17(H17), C19(H19), C22(H22), C25(H25), C26(H26), C27(H27), C28(H28)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Dy1 Dy 0.33737(2) 0.50577(2) 0.44379(2) 0.01398(13) Uani 1 1 d . .
S1 S 0.26197(14) 0.39743(16) 0.77441(14) 0.0388(5) Uani 1 1 d . .
S2 S 0.40035(14) 0.58851(16) 0.96964(13) 0.0370(5) Uani 1 1 d . .
O1 O 0.4062(3) 0.3582(4) 0.5326(3) 0.0241(10) Uani 1 1 d . .
O2 O 0.5741(3) 0.3444(3) 0.5687(3) 0.0229(10) Uani 1 1 d . .
O3 O 0.6860(3) 0.0935(4) 0.9385(3) 0.0285(11) Uani 1 1 d . .
O4 O 0.7519(3) 0.1247(4) 0.8338(3) 0.0310(11) Uani 1 1 d . .
O5 O 0.3817(3) 0.5654(4) 0.5902(3) 0.0233(10) Uani 1 1 d . .
O6 O 0.5478(3) 0.5533(4) 0.6205(3) 0.0281(10) Uani 1 1 d . .
O7 O 0.7115(3) 0.8948(4) 0.8152(3) 0.0268(10) Uani 1 1 d . .
O8 O 0.7142(3) 0.8612(4) 0.9518(3) 0.0267(11) Uani 1 1 d . .
N2 N 0.2134(5) 0.5806(5) 1.1448(5) 0.0470(18) Uani 1 1 d . .
H2 H 0.1802 0.5801 1.1810 0.056 Uiso 1 1 calc R .
N3 N 0.0291(6) 0.4245(7) 0.9108(7) 0.074(3) Uani 1 1 d . .
C1 C 0.4926(4) 0.3354(5) 0.5856(4) 0.0194(13) Uani 1 1 d . .
C2 C 0.5013(4) 0.2945(5) 0.6757(4) 0.0207(13) Uani 1 1 d . .
C3 C 0.4237(5) 0.3143(5) 0.7112(5) 0.0269(15) Uani 1 1 d . .
H3 H 0.3678 0.3535 0.6778 0.032 Uiso 1 1 calc R .
C4 C 0.4296(5) 0.2761(6) 0.7949(5) 0.0287(15) Uani 1 1 d . .
C5 C 0.5138(5) 0.2188(5) 0.8447(4) 0.0223(14) Uani 1 1 d . .
H5 H 0.5181 0.1928 0.9006 0.027 Uiso 1 1 calc R .
C6 C 0.5928(5) 0.1995(5) 0.8123(5) 0.0259(15) Uani 1 1 d . .
C7 C 0.6825(5) 0.1359(5) 0.8666(4) 0.0211(13) Uani 1 1 d . .
C8 C 0.5874(5) 0.2408(5) 0.7293(5) 0.0245(14) Uani 1 1 d . .
H8 H 0.6415 0.2327 0.7095 0.029 Uiso 1 1 calc R .
C9 C 0.3495(5) 0.2959(7) 0.8341(5) 0.0356(18) Uani 1 1 d . .
H9A H 0.3803 0.3180 0.8959 0.043 Uiso 1 1 calc R .
H9B H 0.3135 0.2297 0.8335 0.043 Uiso 1 1 calc R .
C10 C 0.1783(5) 0.4051(6) 0.8318(5) 0.0342(17) Uani 1 1 d . .
C11 C 0.0949(6) 0.4745(7) 0.7950(7) 0.045(2) Uani 1 1 d . .
H11 H 0.0855 0.5133 0.7429 0.054 Uiso 1 1 calc R .
C12 C 0.0281(8) 0.4804(8) 0.8420(9) 0.063(3) Uani 1 1 d . .
H12 H -0.0232 0.5304 0.8215 0.075 Uiso 1 1 calc R .
C13 C 0.1083(7) 0.3609(8) 0.9457(7) 0.059(3) Uani 1 1 d . .
H13 H 0.1144 0.3231 0.9977 0.070 Uiso 1 1 calc R .
C14 C 0.1828(6) 0.3490(6) 0.9067(6) 0.0424(19) Uani 1 1 d . .
H14 H 0.2359 0.3023 0.9322 0.051 Uiso 1 1 calc R .
C15 C 0.4717(4) 0.5851(5) 0.6389(4) 0.0164(12) Uani 1 1 d . .
C16 C 0.4890(4) 0.6509(5) 0.7225(4) 0.0193(13) Uani 1 1 d . .
C17 C 0.4174(4) 0.6472(5) 0.7626(4) 0.0178(12) Uani 1 1 d . .
H17 H 0.3598 0.6063 0.7377 0.021 Uiso 1 1 calc R .
C18 C 0.4312(5) 0.7051(5) 0.8411(4) 0.0198(13) Uani 1 1 d . .
C19 C 0.5166(5) 0.7674(5) 0.8759(4) 0.0223(14) Uani 1 1 d . .
H19 H 0.5262 0.8057 0.9283 0.027 Uiso 1 1 calc R .
C20 C 0.5884(4) 0.7740(5) 0.8345(4) 0.0181(12) Uani 1 1 d . .
C21 C 0.6774(4) 0.8474(5) 0.8700(4) 0.0181(13) Uani 1 1 d . .
C22 C 0.5734(4) 0.7156(5) 0.7562(4) 0.0186(13) Uani 1 1 d . .
H22 H 0.6196 0.7199 0.7267 0.022 Uiso 1 1 calc R .
C23 C 0.3568(5) 0.6973(5) 0.8907(4) 0.0256(14) Uani 1 1 d . .
H23A H 0.2900 0.6824 0.8493 0.031 Uiso 1 1 calc R .
H23B H 0.3551 0.7638 0.9216 0.031 Uiso 1 1 calc R .
C24 C 0.3206(5) 0.5876(5) 1.0306(4) 0.0252(14) Uani 1 1 d . .
C25 C 0.2334(5) 0.6468(5) 1.0120(4) 0.0266(14) Uani 1 1 d . .
H25 H 0.2100 0.6887 0.9607 0.032 Uiso 1 1 calc R .
C26 C 0.1817(5) 0.6419(7) 1.0725(5) 0.041(2) Uani 1 1 d . .
H26 H 0.1238 0.6825 1.0618 0.050 Uiso 1 1 calc R .
C27 C 0.2935(8) 0.5210(7) 1.1626(7) 0.049(2) Uani 1 1 d . .
H27 H 0.3124 0.4781 1.2134 0.058 Uiso 1 1 calc R .
C28 C 0.3497(7) 0.5202(6) 1.1088(5) 0.0385(19) Uani 1 1 d . .
H28 H 0.4061 0.4769 1.1221 0.046 Uiso 1 1 calc R .
O1W O 0.6111(10) 0.9647(10) 1.0701(9) 0.148(4) Uani 1 1 d . U
H1WA H 0.6572 0.9945 1.1124 0.222 Uiso 1 1 d R .
H1WB H 0.6405 0.9331 1.0283 0.222 Uiso 1 1 d 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'
S S 0.1246 0.1234 '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 O3 78.62(15) . 4_565
O1 Dy1 O4 84.77(17) . 4_565
O1 Dy1 O7 155.97(16) . 4_575
O1 Dy1 O8 131.74(15) . 4_575
O1 Dy1 C7 82.48(17) . 4_565
O1 Dy1 C21 150.85(15) . 4_575
O2 Dy1 O1 124.62(15) 3_666 .
O2 Dy1 O3 154.78(15) 3_666 4_565
O2 Dy1 O4 130.17(16) 3_666 4_565
O2 Dy1 O5 81.77(15) 3_666 .
O2 Dy1 O6 74.54(15) 3_666 3_666
O2 Dy1 O7 77.71(15) 3_666 4_575
O2 Dy1 O8 82.76(15) 3_666 4_575
O2 Dy1 C7 149.08(17) 3_666 4_565
O2 Dy1 C21 79.80(16) 3_666 4_575
O3 Dy1 O7 81.50(15) 4_565 4_575
O3 Dy1 C7 26.81(16) 4_565 4_565
O3 Dy1 C21 75.22(17) 4_565 4_575
O4 Dy1 O3 54.06(15) 4_565 4_565
O4 Dy1 O7 72.62(17) 4_565 4_575
O4 Dy1 O8 107.88(16) 4_565 4_575
O4 Dy1 C7 27.36(16) 4_565 4_565
O4 Dy1 C21 90.13(17) 4_565 4_575
O5 Dy1 O1 74.30(15) . .
O5 Dy1 O3 97.53(15) . 4_565
O5 Dy1 O4 148.06(16) . 4_565
O5 Dy1 O7 121.95(15) . 4_575
O5 Dy1 O8 71.55(14) . 4_575
O5 Dy1 C7 123.68(17) . 4_565
O5 Dy1 C21 96.50(16) . 4_575
O6 Dy1 O1 78.67(16) 3_666 .
O6 Dy1 O3 124.20(16) 3_666 4_565
O6 Dy1 O4 73.65(15) 3_666 4_565
O6 Dy1 O5 123.65(15) 3_666 .
O6 Dy1 O7 101.94(16) 3_666 4_575
O6 Dy1 O8 149.41(16) 3_666 4_575
O6 Dy1 C7 99.95(17) 3_666 4_565
O6 Dy1 C21 127.23(17) 3_666 4_575
O7 Dy1 C7 73.72(17) 4_575 4_565
O7 Dy1 C21 26.73(15) 4_575 4_575
O8 Dy1 O3 73.25(16) 4_575 4_565
O8 Dy1 O7 52.46(14) 4_575 4_575
O8 Dy1 C7 89.04(18) 4_575 4_565
O8 Dy1 C21 25.74(15) 4_575 4_575
C7 Dy1 C21 80.0(2) 4_565 4_575
C10 S1 C9 103.5(3) . .
C24 S2 C23 105.2(3) . .
C1 O1 Dy1 134.2(4) . .
C1 O2 Dy1 130.6(4) . 3_666
C7 O3 Dy1 90.4(4) . 4_666
C7 O4 Dy1 92.6(4) . 4_666
C15 O5 Dy1 123.2(4) . .
C15 O6 Dy1 167.9(4) . 3_666
C21 O7 Dy1 90.1(4) . 4_676
C21 O8 Dy1 95.3(4) . 4_676
C27 N2 C26 122.0(7) . .
C12 N3 C13 116.0(8) . .
O1 C1 O2 125.6(6) . .
O1 C1 C2 117.6(5) . .
O2 C1 C2 116.7(5) . .
C3 C2 C1 120.3(6) . .
C8 C2 C1 121.3(5) . .
C8 C2 C3 118.3(6) . .
C4 C3 C2 121.3(6) . .
C3 C4 C9 122.5(6) . .
C5 C4 C3 119.0(6) . .
C5 C4 C9 118.5(6) . .
C4 C5 C6 121.2(6) . .
C5 C6 C7 120.3(6) . .
C8 C6 C5 119.4(6) . .
C8 C6 C7 120.3(6) . .
O3 C7 Dy1 62.8(3) . 4_666
O3 C7 O4 122.4(6) . .
O3 C7 C6 121.1(6) . .
O4 C7 Dy1 60.1(3) . 4_666
O4 C7 C6 116.5(6) . .
C6 C7 Dy1 170.4(5) . 4_666
C6 C8 C2 120.6(6) . .
C4 C9 S1 112.5(5) . .
C11 C10 S1 116.1(6) . .
C14 C10 S1 126.6(6) . .
C14 C10 C11 117.3(7) . .
C12 C11 C10 115.6(9) . .
N3 C12 C11 127.7(9) . .
N3 C13 C14 122.2(9) . .
C10 C14 C13 120.9(8) . .
O5 C15 O6 123.5(5) . .
O5 C15 C16 118.1(5) . .
O6 C15 C16 118.4(5) . .
C17 C16 C15 117.9(5) . .
C17 C16 C22 121.0(6) . .
C22 C16 C15 121.1(5) . .
C16 C17 C18 119.9(6) . .
C17 C18 C23 121.3(6) . .
C19 C18 C17 119.0(5) . .
C19 C18 C23 119.7(5) . .
C18 C19 C20 121.7(6) . .
C19 C20 C21 120.9(5) . .
C19 C20 C22 118.6(6) . .
C22 C20 C21 120.4(5) . .
O7 C21 Dy1 63.2(3) . 4_676
O7 C21 C20 119.3(5) . .
O8 C21 Dy1 59.0(3) . 4_676
O8 C21 O7 122.1(6) . .
O8 C21 C20 118.5(5) . .
C20 C21 Dy1 175.8(4) . 4_676
C16 C22 C20 119.8(5) . .
C18 C23 S2 106.0(4) . .
C25 C24 S2 125.9(5) . .
C25 C24 C28 117.9(6) . .
C28 C24 S2 116.2(5) . .
C24 C25 C26 118.1(6) . .
N2 C26 C25 121.4(7) . .
N2 C27 C28 121.5(8) . .
C27 C28 C24 119.1(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O1 2.324(4) .
Dy1 O2 2.299(4) 3_666
Dy1 O3 2.456(4) 4_565
Dy1 O4 2.396(5) 4_565
Dy1 O5 2.320(4) .
Dy1 O6 2.320(4) 3_666
Dy1 O7 2.536(4) 4_575
Dy1 O8 2.446(4) 4_575
Dy1 C7 2.762(6) 4_565
Dy1 C21 2.842(6) 4_575
S1 C9 1.802(7) .
S1 C10 1.731(7) .
S2 C23 1.810(7) .
S2 C24 1.723(6) .
O1 C1 1.262(7) .
O2 Dy1 2.299(4) 3_666
O2 C1 1.278(7) .
O3 Dy1 2.456(4) 4_666
O3 C7 1.246(7) .
O4 Dy1 2.396(5) 4_666
O4 C7 1.271(7) .
O5 C15 1.271(7) .
O6 Dy1 2.320(4) 3_666
O6 C15 1.277(7) .
O7 Dy1 2.536(4) 4_676
O7 C21 1.278(7) .
O8 Dy1 2.446(4) 4_676
O8 C21 1.239(7) .
N2 C26 1.327(10) .
N2 C27 1.307(10) .
N3 C12 1.295(14) .
N3 C13 1.333(12) .
C1 C2 1.488(8) .
C2 C3 1.420(8) .
C2 C8 1.401(8) .
C3 C4 1.390(9) .
C4 C5 1.385(9) .
C4 C9 1.493(9) .
C5 C6 1.407(9) .
C6 C7 1.499(8) .
C6 C8 1.395(9) .
C7 Dy1 2.762(6) 4_666
C10 C11 1.422(10) .
C10 C14 1.365(11) .
C11 C12 1.397(14) .
C13 C14 1.406(11) .
C15 C16 1.510(8) .
C16 C17 1.374(8) .
C16 C22 1.391(8) .
C17 C18 1.398(8) .
C18 C19 1.387(8) .
C18 C23 1.522(8) .
C19 C20 1.391(8) .
C20 C21 1.506(8) .
C20 C22 1.396(8) .
C21 Dy1 2.842(6) 4_676
C24 C25 1.384(9) .
C24 C28 1.442(10) .
C25 C26 1.398(9) .
C27 C28 1.355(12) .
