Slow relaxation of magnetization and luminescence properties of a novel dysprosium and pyrene-1,3,6,8-tetrasulfonate based MOF
García-García, Amalia; Oyarzabal, Itziar; Cepeda, Javier; Seco, José M.; García-Valdivia, Antonio A.; Gómez-Ruiz, Santiago; Salinas-Castillo, Alfonso; Choquesillo-Lazarte, Duane; Rodríguez-Diéguez, Antonio; New Journal of Chemistry 42 (2018) 832–; doi:10.1039/C7NJ02935G

data_7056751
_publ_section_title
;
 Slow relaxation of magnetization and luminescence properties of a novel
 dysprosium and pyrene-1,3,6,8-tetrasulfonate based MOF
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              832
_journal_paper_doi               10.1039/C7NJ02935G
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety
'C54 H81 Dy2 N10 O29 S6, 2(H2 O), 2(C3 H7 N O)'
_chemical_formula_sum            'C60 H99 Dy2 N12 O33 S6'
_chemical_formula_weight         2033.87
_chemical_name_systematic
'Poly{[diaquatris(mu4-perylene-3,4,9,10-tetracarboxylato)-eicosakis(dimethylformamide)tetradysprosium] tetrahydrate tetrakis(dimethylformamide)}'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-11-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-11-14 deposited with the CCDC.
2017-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.915(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1620(10)
_cell_length_b                   38.224(3)
_cell_length_c                   14.0650(11)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      2.57
_cell_volume                     7585.8(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            160876
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.113
_diffrn_reflns_theta_max         25.113
_diffrn_reflns_theta_min         2.230
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.217
_exptl_absorpt_correction_T_max  0.0111
_exptl_absorpt_correction_T_min  0.0014
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS, Program for Empirical Adsorption Correction, 
Institute for Inorganic Chemistry, University of Gottingen: Germany, 
1996Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_density_method    none
_exptl_crystal_description       'square plate'
_exptl_crystal_F_000             4140
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.024
_refine_diff_density_min         -1.466
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1256
_refine_ls_number_reflns         13454
_refine_ls_number_restraints     444
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+35.5037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1374
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11639
_reflns_number_total             13454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj02935g2.cif
_cod_data_source_block           Compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7056751.cif.
;
_cod_database_code               7056751
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O1M2-C2M2 = O1D2-C2D2 = O1E2-C2E2 = O1J2-C2J2 = O1L2-C2L2
 1.23 with sigma of 0.01
 N3L-C4L = N3L-C5L = N3E-C4E = N3E-C5E = N3J-C4J = N3J-C5J = N3E2-C4E2
 1.45 with sigma of 0.01
 C4J2-C5J2 = C4J-C5J
 2.5 with sigma of 0.01
 C2J2-C4J2
 2.3 with sigma of 0.01
 C2D2-N3D2 = C2M2-N3M2 = C2E2-N3E2 = C2J2-N3J2 = C2L2-N3L2
 1.34 with sigma of 0.01
 O1D-C2D = O1I-C2I = O1L-C2L = O1E-C2E = O1J-C2J = O1M-C2M
 1.23 with sigma of 0.01
 C2D-N3D = C2I-N3I = C2L-N3L = C2E-N3E = C2J-N3J = C2M-N3M
 1.34 with sigma of 0.01
 N3D-C4D = N3D-C5D = N3I-C4I = N3I-C5I = N3M-C4M = N3M-C5M
 1.45 with sigma of 0.01
 N3M2-C4M2 = N3M2-C5M2 = N3D2-C4D2 = N3D2-C5D2 = N3J2-C4J2 = N3J2-C5J2
 1.45 with sigma of 0.01
 C4D-C5D = C4I-C5I = C4L-C5L = C4E-C5E = C4M-C5M = C4M2-C5M2
 2.5 with sigma of 0.01
 N3E2-C5E2 = N3L2-C4L2 = N3L2-C5L2
 1.45 with sigma of 0.01
 N4-C2
 1.36 with sigma of 0.02
 C2-O3
 1.22 with sigma of 0.02
 N4-C5 \\sim N4-C6
 with sigma of 0.02
3. Restrained planarity
 O1D, C2D, N3D, C4D, C5D
 with sigma of 0.1
 O1I, C2I, N3I, C4I, C5I
 with sigma of 0.1
 O1I2, C2I2, N3I2, C4I2, C5I2
 with sigma of 0.1
 O1L, C2L, N3L, C4L, C5L
 with sigma of 0.1
 O1E, C2E, N3E, C4E, C5E
 with sigma of 0.1
 O1M, C2M, N3M, C4M, C5M
 with sigma of 0.1
 O1J, C2J, N3J, C4J, C5J
 with sigma of 0.1
 O1J2, C2J2, N3J2, C4J2, C5J2
 with sigma of 0.1
 O1M2, C2M2, N3M2, C4M2, C5M2
 with sigma of 0.1
 O1L2, C2L2, N3L2, C4L2, C5L2
 with sigma of 0.1
 C2, O3, N4, C5, C6
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O1J \\sim O1J2 \\sim C2J \\sim C2J2 \\sim N3J \\sim N3J2 \\sim C4J \\sim C4J2
\\sim C5J \\sim C5J2: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08
O1L \\sim O1L2 \\sim C2L \\sim C2L2 \\sim N3L \\sim N3L2 \\sim C4L \\sim C4L2
\\sim C5L \\sim C5L2: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08
C2 \\sim O3 \\sim N4 \\sim C5 \\sim C6: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(O3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
5. Rigid body (RIGU) restrains
 C2N, N3N, C4N, C5N
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1M2, C2M2, C5M2, N3M2, C4M2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2, O3, N4, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6, C5, C2, N4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O1M(0.5) C2M(0.5) H2M(0.5) N3M(0.5) C4M(0.5) H4MA(0.5) H4MB(0.5)
 H4MC(0.5) C5M(0.5) H5MA(0.5) H5MB(0.5) H5MC(0.5) O1D(0.5) C2D(0.5) H2D(0.5)
 N3D(0.5) C4D(0.5) H4DA(0.5) H4DB(0.5) H4DC(0.5) C5D(0.5) H5DA(0.5) H5DB(0.5)
 H5DC(0.5) O1E(0.5) C2E(0.5) H2E(0.5) N3E(0.5) C4E(0.5) H4ED(0.5) H4EE(0.5)
 H4EF(0.5) C5E(0.5) H5ED(0.5) H5EE(0.5) H5EF(0.5) O1N(0.5) C2N(0.5) H2N(0.5)
 N3N(0.5) C4N(0.5) H4NA(0.5) H4NB(0.5) H4NC(0.5) C5N(0.5) H5NA(0.5) H5NB(0.5)
 H5NC(0.5) O1I(0.5) C2I(0.5) H2I(0.5) N3I(0.5) C4I(0.5) H4IA(0.5) H4IB(0.5)
 H4IC(0.5) C5I(0.5) H5IA(0.5) H5IB(0.5) H5IC(0.5) O1J(0.5) C2J(0.5) H2J(0.5)
 N3J(0.5) C4J(0.5) H4JA(0.5) H4JB(0.5) H4JC(0.5) C5J(0.5) H5JA(0.5) H5JB(0.5)
 H5JC(0.5) O1L(0.5) C2L(0.5) H2L(0.5) N3L(0.5) C4L(0.5) H4LA(0.5) H4LB(0.5)
 H4LC(0.5) C5L(0.5) H5LA(0.5) H5LB(0.5) H5LC(0.5) O1E2(0.5) C2E2(0.5) H2E2(0.5)
 N3E2(0.5) C4E2(0.5) H4EA(0.5) H4EB(0.5) H4EC(0.5) C5E2(0.5) H5EA(0.5)
 H5EB(0.5) H5EC(0.5) O1D2(0.5) C2D2(0.5) H2D2(0.5) N3D2(0.5) C4D2(0.5)
 H4DD(0.5) H4DE(0.5) H4DF(0.5) C5D2(0.5) H5DD(0.5) H5DE(0.5) H5DF(0.5)
 O1M2(0.5) C2M2(0.5) H2M2(0.5) N3M2(0.5) C4M2(0.5) H4MD(0.5) H4ME(0.5)
 H4MF(0.5) C5M2(0.5) H5MD(0.5) H5ME(0.5) H5MF(0.5) O1I2(0.5) C2I2(0.5)
 H2I2(0.5) N3I2(0.5) C4I2(0.5) H4ID(0.5) H4IE(0.5) H4IF(0.5) C5I2(0.5)
 H5ID(0.5) H5IE(0.5) H5IF(0.5) O1J2(0.5) C2J2(0.5) H2J2(0.5) N3J2(0.5)
 C4J2(0.5) H4JD(0.5) H4JE(0.5) H4JF(0.5) C5J2(0.5) H5JD(0.5) H5JE(0.5)
 H5JF(0.5) O1L2(0.5) C2L2(0.5) H2L2(0.5) N3L2(0.5) C4L2(0.5) H4LD(0.5)
 H4LE(0.5) H4LF(0.5) C5L2(0.5) H5LD(0.5) H5LE(0.5) H5LF(0.5)
7.a Everything fixed:
 H1WA, H1WB
7.b Riding coordinates:
 C4M2(H4MD,H4ME,H4MF), C4L2(H4LD,H4LE,H4LF), C6(H6C,H6D,H6E)
7.c Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C2B(H2B), C5A(H5A), C5B(H5B), C6A(H6A), C6B(H6B), C9A(H9A),
 C12A(H12A), C13A(H13A), C2F(H2F), C2G(H2G), C2H(H2H), C2M(H2M), C2D(H2D),
 C2E(H2E), C2N(H2N), C2I(H2I), C2J(H2J), C2L(H2L), C2E2(H2E2), C2D2(H2D2),
 C2M2(H2M2), C2I2(H2I2), C2J2(H2J2), C2L2(H2L2), C2(H2)
7.d Idealised Me refined as rotating group:
 C4F(H4FA,H4FB,H4FC), C5F(H5FA,H5FB,H5FC), C4G(H4GA,H4GB,H4GC), C5G(H5GA,H5GB,
 H5GC), C4H(H4HA,H4HB,H4HC), C5H(H5HA,H5HB,H5HC), C4M(H4MA,H4MB,H4MC), C5M(H5MA,
 H5MB,H5MC), C4D(H4DA,H4DB,H4DC), C5D(H5DA,H5DB,H5DC), C4E(H4ED,H4EE,H4EF),
 C5E(H5ED,H5EE,H5EF), C4N(H4NA,H4NB,H4NC), C5N(H5NA,H5NB,H5NC), C4I(H4IA,H4IB,
 H4IC), C5I(H5IA,H5IB,H5IC), C4J(H4JA,H4JB,H4JC), C5J(H5JA,H5JB,H5JC), C4L(H4LA,
 H4LB,H4LC), C5L(H5LA,H5LB,H5LC), C4E2(H4EA,H4EB,H4EC), C5E2(H5EA,H5EB,H5EC),
 C4D2(H4DD,H4DE,H4DF), C5D2(H5DD,H5DE,H5DF), C5M2(H5MD,H5ME,H5MF), C4I2(H4ID,
 H4IE,H4IF), C5I2(H5ID,H5IE,H5IF), C4J2(H4JD,H4JE,H4JF), C5J2(H5JD,H5JE,H5JF),
 C5L2(H5LD,H5LE,H5LF), C5(H5C,H5D,H5E)
;
_shelx_res_checksum              89760
_olex2_submission_special_instructions 'No special instructions were received'