Slow relaxation of the magnetization, reversible solvent exchange and luminescence in 2D anilato-based frameworks.
Benmansour, Samia; Hernández-Paredes, Antonio; Mondal, Arpan; López Martínez, Gustavo; Canet-Ferrer, Josep; Konar, Sanjit; Gómez-García, Carlos J; Chemical communications (Cambridge, England) 56 (2020) 9862–9865; doi:10.1039/d0cc03964k

data_7126935
_publ_section_title
;
 Slow relaxation of the magnetization, reversible solvent exchange and
 luminescence in 2D anilato-based frameworks.
;
_journal_issue                   68
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9862
_journal_page_last               9865
_journal_paper_doi               10.1039/d0cc03964k
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C18 H21 Br3 Dy N3 O9'
_chemical_formula_sum            'C18 H21 Br3 Dy N3 O9'
_chemical_formula_weight         825.61
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-22 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.859(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0215(5)
_cell_length_b                   13.4454(6)
_cell_length_c                   19.4727(9)
_cell_measurement_reflns_used    3968
_cell_measurement_temperature    119.7(9)
_cell_measurement_theta_max      24.9360
_cell_measurement_theta_min      3.6440
_cell_volume                     2610.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.7(9)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -91.00 -35.00   1.00   37.50    --  -14.89-178.00 -60.00   56
  2  \w    -59.00  58.00   1.00   37.50    --  -14.89  19.00-180.00  117
  3  \w    -87.00  11.00   1.00   37.50    --  -14.89 -38.00 150.00   98
  4  \w    -20.00   5.00   1.00   37.50    --  -14.89 -99.00  60.00   25
  5  \w    -36.00  34.00   1.00   37.50    --  -14.89  57.00 -90.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0578723000
_diffrn_orient_matrix_UB_12      -0.0306635000
_diffrn_orient_matrix_UB_13      -0.0039786000
_diffrn_orient_matrix_UB_21      0.0008631000
_diffrn_orient_matrix_UB_22      -0.0031896000
_diffrn_orient_matrix_UB_23      0.0364019000
_diffrn_orient_matrix_UB_31      -0.0413881000
_diffrn_orient_matrix_UB_32      0.0428048000
_diffrn_orient_matrix_UB_33      -0.0001477000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_av_unetI/netI     0.0789
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17018
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.056
_diffrn_reflns_theta_max         25.056
_diffrn_reflns_theta_min         3.431
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.505
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41q (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.101
_exptl_crystal_description       block
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.364
_refine_diff_density_min         -1.312
_refine_diff_density_rms         0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         4602
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0662
_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/[\s^2^(Fo^2^)+(0.0711P)^2^+39.7467P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1603
_refine_ls_wR_factor_ref         0.1727
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3575
_reflns_number_total             4602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03964k2.cif
_cod_data_source_block           crys333a
_cod_depositor_comments
'Adding full bibliography for 7126934--7126936.cif.'
_cod_database_code               7126935
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.753
_shelx_estimated_absorpt_t_min   0.442
_reflns_odcompleteness_completeness 86.33
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
2. Restrained distances
 N11D-C13D \\sim N1D-C2D \\sim N21D-C22D
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1D) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of
0.0004 and sigma for terminal atoms of 0.0008
Uanis(O12) \\sim Ueq: with sigma of 0.0004 and sigma for terminal atoms of
0.0008
Uanis(C2D) \\sim Ueq, Uanis(C3D) \\sim Ueq: with sigma of 0.0004 and sigma for
terminal atoms of 0.0008
Uanis(C12D) \\sim Ueq, Uanis(C13D) \\sim Ueq: with sigma of 0.0004 and sigma
for terminal atoms of 0.0008
Uanis(C22D) \\sim Ueq, Uanis(C23D) \\sim Ueq: with sigma of 0.0004 and sigma
for terminal atoms of 0.0008
Uanis(C4) \\sim Ueq: with sigma of 0.0004 and sigma for terminal atoms of 0.0008
Uanis(C1) \\sim Ueq: with sigma of 0.0004 and sigma for terminal atoms of 0.0008
Uanis(C11D) \\sim Ueq, Uanis(C21D) \\sim Ueq: with sigma of 0.0004 and sigma
for terminal atoms of 0.0008
Uanis(C1D) \\sim Ueq: with sigma of 0.0004 and sigma for terminal atoms of
0.0008
Uanis(N1D) \\sim Ueq: with sigma of 0.0004 and sigma for terminal atoms of
0.0008
Uanis(O21D) \\sim Ueq: with sigma of 0.0004 and sigma for terminal atoms of
0.0008
Uanis(N21D) \\sim Ueq: with sigma of 0.0004 and sigma for terminal atoms of
0.0008
4.a Me refined with riding coordinates:
 C2D(H2DA,H2DB,H2DC), C3D(H3DA,H3DB,H3DC), C12D(H12A,H12B,H12C), C13D(H13A,
 H13B,H13C), C23D(H23A,H23B,H23C)
4.b Aromatic/amide H refined with riding coordinates:
 C1D(H1D), C11D(H11D), C21D(H21D)
4.c Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6)
4.d Idealised Me refined as rotating group:
 C22D(H22A,H22B,H22C)
;
_shelx_res_checksum              62627
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop usin paratone oil'
_olex2_submission_original_sample_id AH188
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.401
_oxdiff_exptl_absorpt_empirical_full_min 0.724