Enhancing the energy barrier and hysteresis temperature in two benchtop-stable Ho(iii) single-ion magnets.
Jia, Kexin; Meng, Xixi; Wang, Mengmeng; Gou, Xiaoshuang; Wang, Yu-Xia; Xu, Na; Shi, Wei; Cheng, Peng; Chemical communications (Cambridge, England) 57 (2021) 3607–3610; doi:10.1039/d1cc00582k

data_7128006
_publ_section_title
;
 Enhancing the energy barrier and hysteresis temperature in two
 benchtop-stable Ho(iii) single-ion magnets.
;
_journal_issue                   29
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3607
_journal_page_last               3610
_journal_paper_doi               10.1039/d1cc00582k
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C24 H60 Cl3 Ho N6 O8 P2'
_chemical_formula_sum            'C24 H60 Cl3 Ho N6 O8 P2'
_chemical_formula_weight         894.00
_chemical_name_systematic        'Ho(tppo)2(H2O)5Cl3 H2O'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2021-01-29 deposited with the CCDC.	2021-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.9663(3)
_cell_length_b                   26.9370(9)
_cell_length_c                   30.2924(9)
_cell_measurement_reflns_used    9137
_cell_measurement_temperature    293
_cell_measurement_theta_max      24.9670
_cell_measurement_theta_min      2.2730
_cell_volume                     8132.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_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      293
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     32.00 109.00   0.50   12.00    --   20.00  54.00-180.00  154
  2  \w    -55.00 -29.00   0.50   12.00    --   20.00  54.00  30.00   52
  3  \w    -27.00   0.00   0.50   12.00    --   20.00  54.00  30.00   54
  4  \w     69.00 100.00   0.50   12.00    --   20.00  54.00  30.00   62
  5  \w    -72.00 106.00   0.50   12.00    --   20.00  54.00   0.00  356
  6  \w    -67.00 -42.00   0.50   12.00    --   20.00  54.00  90.00   50
  7  \w     12.00  55.00   0.50   12.00    --   20.00  54.00  90.00   86
  8  \w      1.00  26.00   0.50   12.00    --   20.00  54.00-180.00   50
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0095712000
_diffrn_orient_matrix_UB_12      -0.0258824000
_diffrn_orient_matrix_UB_13      0.0030054000
_diffrn_orient_matrix_UB_21      -0.0222672000
_diffrn_orient_matrix_UB_22      0.0043354000
_diffrn_orient_matrix_UB_23      0.0219047000
_diffrn_orient_matrix_UB_31      -0.0668983000
_diffrn_orient_matrix_UB_32      0.0022385000
_diffrn_orient_matrix_UB_33      -0.0077072000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            43248
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.655
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.267
_exptl_absorpt_correction_T_max  0.69235
_exptl_absorpt_correction_T_min  0.62499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pinkish pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             3664
_exptl_crystal_preparation       NONE
_exptl_crystal_recrystallization_method NONE
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.627
_refine_diff_density_min         -1.467
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         7173
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0601P)^2^+39.5145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1461
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4953
_reflns_number_total             7173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00582k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7128006--7128007.cif.'
_cod_database_code               7128006
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_usercomment     'C H O Dy'
_reflns_odcompleteness_completeness 86.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O5-H5b \\sim O1-H1a
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C0AA \\sim C18 \\sim C20: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C10) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5.a Free rotating group:
 O8(H8c,H8d)
5.b Rotating group:
 O1(H1a), O2(H2a), O3(H3a), O5(H5a)
5.c Secondary CH2 refined with riding coordinates:
 C1(H1c,H1d), C2(H2c,H2d), C3(H3c,H3d), C4(H4c,H4d), C5(H5c,H5d), C6(H6a,H6b),
 C7(H7a,H7b), C8(H8a,H8b), C9(H9a,H9b), C10(H10a,H10b), C11(H11a,H11b),
 C12(H12a,H12b), C13(H13a,H13b), C14(H14a,H14b), C15(H15a,H15b), C16(H16a,H16b),
  C17(H17a,H17b), C18(H18a,H18b), C20(H20a,H20b), C21(H21a,H21b), C22(H22a,
 H22b), C23(H23a,H23b), C24(H24a,H24b), C0AA(H0Aa,H0Ab)
;
_shelx_res_checksum              37579
_olex2_exptl_crystal_mounting_method 293
_olex2_submission_original_sample_id Ho-Cl
_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 1.524
_oxdiff_exptl_absorpt_empirical_full_min 0.786