Chemical and in silico tuning of the magnetisation reversal barrier in pentagonal bipyramidal Dy(iii) single-ion magnets.
Canaj, Angelos B.; Singh, Mukesh Kumar; Wilson, Claire; Rajaraman, Gopalan; Murrie, Mark; Chemical communications (Cambridge, England) 54 (2018) 8273–8276; doi:10.1039/c8cc03929a

data_7121941
_publ_section_title
;
 Chemical and in silico tuning of the magnetisation reversal barrier in
 pentagonal bipyramidal Dy(iii) single-ion magnets.
;
_journal_issue                   59
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8273
_journal_page_last               8276
_journal_paper_doi               10.1039/c8cc03929a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C12 H46 Dy N6 O7 P2, 3(I), 2(C6 H18 N3 O P)'
_chemical_formula_sum            'C24 H82 Dy I3 N12 O9 P4'
_chemical_formula_weight         1350.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-04-06 deposited with the CCDC.
2018-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.075(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0512(7)
_cell_length_b                   19.1355(10)
_cell_length_c                   20.4829(11)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.459
_cell_measurement_theta_min      2.357
_cell_volume                     5404.8(5)
_computing_cell_refinement       'SAINT V8.37A (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'charge integrating pixel array detector'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  Photon
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24453
_diffrn_reflns_point_group_measured_fraction_full 0.920
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         2.358
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.263
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1249 before and 0.0582 after correction. The Ratio of minimum to maximum transmission is 0.8946. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_description       block
_exptl_crystal_F_000             2668
_exptl_crystal_size_max          0.139
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.168
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 4376 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.004(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         11023
_refine_ls_number_restraints     531
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0241
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0536
_reflns_Friedel_coverage         0.786
_reflns_Friedel_fraction_full    0.841
_reflns_Friedel_fraction_max     0.784
_reflns_number_gt                10586
_reflns_number_total             11023
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03929a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7121940--7121943.cif.'
_cod_database_code               7121941
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.660
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O3W-H3WB = O3W-H3WA = O2W-H2WB = O2W-H2WA = O1W-H1WB = O1W-H1WA = O4W-H4WB =
 O4W-H4WA = O5W-H5WB = O5W-H5WA
 0.85 with sigma of 0.02
 N12A-C17A \\sim N12A-C18 \\sim N12-C18 \\sim N12-C17 \\sim N11A-C15A \\sim
N11A-C16 \\sim N11-C15 ~
 N11-C16 \\sim N10A-C14A \\sim N10A-C13 \\sim N10-C13 \\sim N10-C14
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(H18D)=
 Sof(H18E)=Sof(H18F)=Sof(N10A)=Sof(N11A)=Sof(N12A)=Sof(C14A)=Sof(H14D)=
 Sof(H14E)=Sof(H14F)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C17A)=
 Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(N10)=Sof(N11)=Sof(N12)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=
 Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(H18A)=Sof(H18B)=Sof(H18C)=
 FVAR(1)
5.a Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C13(H13D,H13E,H13F), C16(H16A,H16B,H16C), C16(H16D,H16E,
 H16F), C18(H18A,H18B,H18C), C18(H18D,H18E,H18F)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C24(H24A,H24B,H24C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C17(H17A,H17B,H17C), C14A(H14D,H14E,H14F), C15A(H15D,H15E,H15F), C17A(H17D,
 H17E,H17F)
;
_shelx_res_checksum              63510
_olex2_submission_special_instructions 'No special instructions were received'