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_7047526
_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 H7 Dy N2 O8, 1.76(H2 O)'
_chemical_formula_sum            'C16 H10.52 Dy N2 O9.76'
_chemical_formula_weight         549.44
_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
_atom_sites_solution_primary     dual
_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
;
2018-08-20 deposited with the CCDC.
2018-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                109.487(3)
_cell_angle_beta                 90.285(2)
_cell_angle_gamma                92.121(3)
_cell_formula_units_Z            2
_cell_length_a                   7.1771(2)
_cell_length_b                   9.0830(3)
_cell_length_c                   13.2629(4)
_cell_measurement_reflns_used    3480
_cell_measurement_temperature    119.9(3)
_cell_measurement_theta_max      26.1730
_cell_measurement_theta_min      3.2380
_cell_volume                     814.38(5)
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_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    -83.00   7.00   1.00   40.00    --  -15.64 -63.00-159.68   90
  2  \w    -84.00   6.00   1.00   40.00    --  -15.64 -57.00 -90.00   90
  3  \w    -84.00   9.00   1.00   40.00    --  -15.64 -69.00  19.11   93
  4  \w    -84.00   6.00   1.00   40.00    --  -15.64 -57.00  90.00   90
  5  \w    -53.00  38.00   1.00   40.00    --   16.26 -57.00-120.00   91
  6  \w    -50.00  43.00   1.00   40.00    --   18.00 -69.00  -9.07   93
  7  \w    -51.00  44.00   1.00   40.00    --   18.00 -70.00 164.73   95
  8  \w    -51.00  44.00   1.00   40.00    --   18.00 -70.00  95.08   95
  9  \w    -52.00   3.00   1.00   40.00    --   16.26 -69.00 -47.12   55
;
_diffrn_measurement_device       'four-circle diffractometer'
_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      -0.0362743000
_diffrn_orient_matrix_UB_12      -0.0684883000
_diffrn_orient_matrix_UB_13      0.0085635000
_diffrn_orient_matrix_UB_21      -0.0714725000
_diffrn_orient_matrix_UB_22      0.0436214000
_diffrn_orient_matrix_UB_23      0.0317226000
_diffrn_orient_matrix_UB_31      -0.0579617000
_diffrn_orient_matrix_UB_32      -0.0167314000
_diffrn_orient_matrix_UB_33      -0.0462569000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11040
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         2.841
_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              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.653
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.845
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.241
_exptl_crystal_description       block
_exptl_crystal_F_000             529
_exptl_crystal_size_max          0.044
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.021
_refine_diff_density_max         1.223
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         2785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0385
_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/[\s^2^(Fo^2^)+(0.0303P)^2^+0.4558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0806
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2455
_reflns_number_total             2785
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03421d2.cif
_cod_data_source_block           dy-jc23a11-125c-a_ref3
_cod_depositor_comments
'Adding full bibliography for 7047525--7047526.cif.'
_cod_database_code               7047526
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Dy C16 H6 O8 N2'
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.821
_reflns_odcompleteness_completeness 99.89
_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
2. Uiso/Uaniso restraints and constraints
Uanis(C12) = Uanis(C22)
Uanis(O1) = Uanis(O172)
Uanis(O1W) = Uanis(O1WA)
3. Others
 Sof(O1)=Sof(H1)=1-FVAR(1)
 Sof(O172)=Sof(H172)=FVAR(1)
 Sof(O1WA)=Sof(H1WC)=Sof(H1WD)=1-FVAR(2)
 Sof(O1W)=Sof(H1WA)=Sof(H1WB)=FVAR(2)
 Fixed Sof: O2W(0.3) H2WA(0.3) H2WB(0.3) O2WA(0.46) H2WC(0.46) H2WD(0.46)
4.a Free rotating group:
 O2W(H2WA,H2WB,O2WA,H2WC,H2WD)
4.b :
 O1W(H1WA,H1WB,O1WA,H1WC,H1WD)
4.c Aromatic/amide H refined with riding coordinates:
 C42(H42), C41(H41), C61(H61), C62(H62), C21(H21), C22(H22)
4.d Idealised tetrahedral OH refined as rotating group:
 O172(H172), O1(H1)
;
_shelx_res_checksum              28230
_olex2_submission_original_sample_id MUV-4b
_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 1.158
_oxdiff_exptl_absorpt_empirical_full_min 0.873