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_7121940
_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(Cl), C6 H18 N3 O P, H2 O'
_chemical_formula_sum            'C18 H66 Cl3 Dy N9 O9 P3'
_chemical_formula_weight         914.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-07-14
_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                 101.025(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.3237(10)
_cell_length_b                   38.167(4)
_cell_length_c                   19.4676(18)
_cell_measurement_reflns_used    9693
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.482
_cell_measurement_theta_min      2.512
_cell_volume                     8258.4(14)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_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 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_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  0.0329
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            97180
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_min         2.197
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.168
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0726 before and 0.0503 after correction. The Ratio of minimum to maximum transmission is 0.8743. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       prism
_exptl_crystal_F_000             3768
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.897
_refine_diff_density_min         -1.352
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     942
_refine_ls_number_reflns         18913
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+10.6412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0538
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17718
_reflns_number_total             18913
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03929a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7121940--7121943.cif.'
_cod_original_cell_volume        8258.4(13)
_cod_database_code               7121940
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.812
_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
 H6WA-O6W
 0.85 with sigma of 0.02
 O1S-H1SB
 0.85 with sigma of 0.02
 N12-C24 \\sim N12-C23 \\sim N120-C240 \\sim N110-C220 \\sim N110-C210 \\sim
N11-C22 \\sim N11-C21 ~
 N100-C190 \\sim N100-C20 \\sim N10-C20 \\sim N10-C19 \\sim N121-C231 \\sim
N121-C241 \\sim N120-C230
 with sigma of 0.02
3. Others
 Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(N100)=Sof(N110)=Sof(C190)=Sof(H19D)=
 Sof(H19E)=Sof(H19F)=Sof(C210)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C220)=
 Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(1)
 Sof(N120)=Sof(C240)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C230)=Sof(H23D)=
 Sof(H23E)=Sof(H23F)=Sof(C231)=Sof(H23G)=Sof(H23H)=Sof(H23I)=Sof(C241)=
 Sof(H24G)=Sof(H24H)=Sof(H24I)=Sof(N121)=0.5*(1-FVAR(2))
 Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(N10)=Sof(N11)=Sof(N12)=Sof(C19)=Sof(H19A)=
 Sof(H19B)=Sof(H19C)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22)=Sof(H22A)=
 Sof(H22B)=Sof(H22C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=
 Sof(H24B)=Sof(H24C)=FVAR(1)
 Fixed Sof: Cl4(0.75) Cl40(0.25)
4.a Free rotating group:
 O2S(H2SA,H2SB)
4.b Me refined with riding coordinates:
 C20(H20A,H20B,H20C), C20(H20D,H20E,H20F)
4.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,
 H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C240(H24D,H24E,H24F), C190(H19D,H19E,H19F), C210(H21D,H21E,H21F), C220(H22D,
 H22E,H22F), 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(H10C,H10D,H10E), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C), C230(H23D,H23E,H23F), C231(H23G,H23H,H23I), C241(H24G,
 H24H,H24I)
;
_shelx_res_checksum              69908
_olex2_submission_special_instructions 'No special instructions were received'