A large barrier single-molecule magnet without magnetic memory.
Giansiracusa, Marcus J.; Al-Badran, Susan; Kostopoulos, Andreas K.; Whitehead, George F. S.; Collison, David; Tuna, Floriana; Winpenny, Richard E. P.; Chilton, Nicholas F.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 10795–10798; doi:10.1039/c9dt01791g

data_7700350
_publ_section_title
;
 A large barrier single-molecule magnet without magnetic memory.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10795
_journal_page_last               10798
_journal_paper_doi               10.1039/c9dt01791g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C22 H24 Cl3 Dy N2 O3'
_chemical_formula_sum            'C22 H24 Cl3 Dy N2 O3'
_chemical_formula_weight         633.28
_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             2018-08-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-28 deposited with the CCDC.    2019-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                110.136(10)
_cell_angle_beta                 106.175(9)
_cell_angle_gamma                92.705(8)
_cell_formula_units_Z            1
_cell_length_a                   7.1829(6)
_cell_length_b                   9.3204(10)
_cell_length_c                   10.2330(13)
_cell_measurement_reflns_used    1593
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      25.4160
_cell_measurement_theta_min      3.7000
_cell_volume                     609.91(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_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      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3271
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_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    -11.00  76.00   1.00   22.43    --   11.22  77.00-180.00   87
  2  \w    -35.00  60.00   1.00   22.43    --  -11.85  57.00  60.00   95
  3  \w    -78.00  13.00   1.00   22.43    --  -11.85 -57.00 -90.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0155165000
_diffrn_orient_matrix_UB_12      -0.0760986000
_diffrn_orient_matrix_UB_13      -0.0364578000
_diffrn_orient_matrix_UB_21      0.0078088000
_diffrn_orient_matrix_UB_22      -0.0165631000
_diffrn_orient_matrix_UB_23      0.0638060000
_diffrn_orient_matrix_UB_31      -0.1026789000
_diffrn_orient_matrix_UB_32      -0.0259733000
_diffrn_orient_matrix_UB_33      -0.0254526000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.1178
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4347
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.363
_diffrn_reflns_theta_min         3.503
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.417
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45i (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_description       plate
_exptl_crystal_F_000             311
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0266P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1774
_reflns_number_total             2475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01791g2.cif
_cod_data_source_block           orgp353sf1
_cod_depositor_comments          'Adding full bibliography for 7700350.cif.'
_cod_original_cell_volume        609.91(12)
_cod_database_code               7700350
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.663
_reflns_odcompleteness_completeness 99.36
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: Cl2(0.5) O2(0.5) H2A(0.5) H2B(0.5)
3.a Riding coordinates:
 O2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C4(H4), C9(H9), C10(H10), C11(H11)
3.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              66770
_olex2_date_sample_data_collection 2016-12-09
_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 1.270
_oxdiff_exptl_absorpt_empirical_full_min 0.918