Implementation of slow magnetic relaxation in a SIM-MOF through a structural rearrangement.
Castells-Gil, Javier; Baldoví, José J; Martí-Gastaldo, Carlos; Mínguez Espallargas, Guillermo; Dalton transactions (Cambridge, England : 2003) 47 (2018) 14734–14740; doi:10.1039/c8dt03421d

data_7047525
_publ_section_title
;
 Implementation of slow magnetic relaxation in a SIM-MOF through a
 structural rearrangement.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14734
_journal_page_last               14740
_journal_paper_doi               10.1039/c8dt03421d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C16 H11 Dy N2 O10, 1.7(H2 O1)'
_chemical_formula_sum            'C16 H14.41 Dy N2 O11.7'
_chemical_formula_weight         584.48
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-11 deposited with the CCDC.
2018-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                74.983(4)
_cell_angle_beta                 78.546(4)
_cell_angle_gamma                83.143(4)
_cell_formula_units_Z            2
_cell_length_a                   6.6676(3)
_cell_length_b                   10.1303(5)
_cell_length_c                   13.8039(6)
_cell_measurement_reflns_used    6247
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      27.0780
_cell_measurement_theta_min      3.1070
_cell_volume                     880.33(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -17.00  51.00   1.00    1.00    --  -17.21  57.00   0.00   68
  2  \w     47.00  80.00   1.00    1.00    --   17.92  57.00  30.00   33
  3  \w      4.00  50.00   1.00    1.00    --  -17.21  57.00-120.00   46
  4  \w     46.00  95.00   1.00    1.00    --   17.92 178.00  30.00   49
  5  \w    -48.00  32.00   1.00    1.00    --   17.92 -57.00  90.00   80
  6  \w     25.00  63.00   1.00    1.00    --   17.92 -99.00  30.00   38
  7  \w    -20.00  63.00   1.00    1.00    --   17.92 -99.00-150.00   83
  8  \w    -83.00  14.00   1.00    1.00    --  -17.21 -73.00 -36.00   97
  9  \w    -88.00   5.00   1.00    1.00    --  -17.21 -57.00  90.00   93
 10  \w    -88.00  -4.00   1.00    1.00    --  -17.21 -57.00-150.00   84
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0530828000
_diffrn_orient_matrix_UB_12      -0.0409678000
_diffrn_orient_matrix_UB_13      0.0383400000
_diffrn_orient_matrix_UB_21      -0.0863317000
_diffrn_orient_matrix_UB_22      -0.0394086000
_diffrn_orient_matrix_UB_23      0.0208563000
_diffrn_orient_matrix_UB_31      0.0396389000
_diffrn_orient_matrix_UB_32      -0.0452893000
_diffrn_orient_matrix_UB_33      -0.0318531000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9519
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.711
_diffrn_reflns_theta_max         24.711
_diffrn_reflns_theta_min         2.886
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.319
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_T_min  0.640
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.205
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_preparation       'Magnetic properties,Luminescent'
_exptl_crystal_recrystallization_method Hydrothermal
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.0008(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         2996
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0262
_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/[\s^2^(Fo^2^)+(0.0133P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0573
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2803
_reflns_number_total             2996
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03421d2.cif
_cod_data_source_block           jc-23a11a_ref
_cod_depositor_comments
'Adding full bibliography for 7047525--7047526.cif.'
_cod_original_formula_sum        'C16 H14.41 Dy N2 O11.70'
_cod_database_code               7047525
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Dy C16 N2 O12 H14'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups, All O(H,H,H) groups
2. Restrained distances
 O2W-H2WA = O2W-H2WB
 0.85 with sigma of 0.02
 O1W-H1WA = O1W-H1WB
 0.85 with sigma of 0.02
 O4W-H4WA = O4W-H4WB
 0.85 with sigma of 0.02
 O3W-H3WA
 0.85 with sigma of 0.02
 O3W-H3WB
 0.85 with sigma of 0.02
 O3W-H3W
 0.85 with sigma of 0.02
 H2WA-H2WB
 1.34 with sigma of 0.04
 H1WA-H1WB
 1.34 with sigma of 0.04
 H4WA-H4WB
 1.34 with sigma of 0.04
 H3WA-H3WB
 1.34 with sigma of 0.04
 H3W-H3WB
 1.34 with sigma of 0.04
 Dy1-H2WA \\sim Dy1-H2WB
 with sigma of 0.02
 Dy1-H1WA \\sim Dy1-H1WB
 with sigma of 0.02
 O3W-H3WA \\sim O3W-H3W
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C71) = Uanis(C31)
4. Others
 Sof(H3W)=1-FVAR(1)
 Sof(H3WA)=FVAR(1)
 Fixed Sof: O4W(0.7) H4WA(0.7) H4WB(0.7)
5.a Free rotating group:
 H3WA(H3WB)
5.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C21(H21), C42(H42), C22(H22), C61(H61), C62(H62)
5.c Idealised tetrahedral OH refined as rotating group:
 O181(H181)
;
_shelx_res_checksum              14028
_olex2_submission_original_sample_id MUV-4a
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.678
_oxdiff_exptl_absorpt_empirical_full_min 0.643