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_7121943
_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 N6 O7 P2 Y), 3(Cl), (C6 H18 N3 O P), (H2 O)'
_chemical_formula_sum            'C18 H66 Cl3 N9 O9 P3 Y'
_chemical_formula_weight         840.96
_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             2018-01-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-06 deposited with the CCDC.
2018-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.936(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.4154(7)
_cell_length_b                   38.613(3)
_cell_length_c                   19.9862(13)
_cell_measurement_reflns_used    9837
_cell_measurement_temperature    298
_cell_measurement_theta_max      26.17
_cell_measurement_theta_min      2.35
_cell_volume                     8619.1(10)
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298
_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 0.999
_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  0.0541
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       49
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            94898
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.464
_diffrn_reflns_theta_min         2.149
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.697
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0603 before and 0.0482 after correction. The Ratio of minimum to maximum transmission is 0.9083. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       prism
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     892
_refine_ls_number_reflns         19662
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0509P)^2^+6.4546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1233
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13854
_reflns_number_total             19662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03929a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7121940--7121943.cif.'
_cod_original_cell_volume        8619.2(10)
_cod_database_code               7121943
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.773
_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
2. Restrained distances
 O10-H10E = O10-H10D = O11-H11D = O11-H11E = O12-H12E = O12-H12D = O13-H13A =
 O13-H13B = O14-H14A
 0.85 with sigma of 0.02
 O2S-H2SA = O2S-H2SB
 0.85 with sigma of 0.02
 O1S-H1SA = O1S-H1SB
 0.85 with sigma of 0.02
 O6-H6A = O6-H6B = O7-H7B = O7-H7A = O8-H8A = O8-H8B = O9-H9B = O9-H9A
 0.85 with sigma of 0.02
 O14-H14B
 0.85 with sigma of 0.02
 N1-C1
 1.469 with sigma of 0.005
 O5-H5B = O5-H5A
 0.85 with sigma of 0.02
 N2-C5A
 1.469 with sigma of 0.02
 N18-C35 = N18-C36 = N17-C33 = N17-C34 = N16-C32 = N16-C31 = N14-C29 = N14-C30
 = N13-C25 = N13-C26 = N15-C27 = N15-C28 = N4-C8 = N4-C7 = N5-C11 = N5-C12 = N6-
 C9 = N6-C10 = N2-C6 = N2-C5 = N1-C1 = N1-C2 = N1A-C2A = N3-C3 = N3-C4 = N3A-
 C3A = N3A-C4A = N9-C16 = N9-C15A = N9-C15 = N7-C18A = N7-C17 = N7-C18 = N10-
 C23 = N10-C24 = N11-C19 = N11-C20 = N12-C21 = N12-C22 = N1A-C1 = N1-C1
 1.469 with sigma of 0.01
 C1-C2 \\sim C1-C2A
 with sigma of 0.02
3. Others
 Fixed Sof: N1A(0.6) N3(0.4) H1BD(0.6) H1BE(0.6) H1BF(0.6) H1AA(0.4) H1AB(0.4)
 H1AC(0.4) C2A(0.6) H2AA(0.6) H2AB(0.6) H2AC(0.6) C3(0.4) H3A(0.4) H3B(0.4)
 H3C(0.4) C4(0.4) H4A(0.4) H4B(0.4) H4C(0.4) C5(0.6) H5C(0.6) H5D(0.6) H5E(0.6)
 C15(0.6) H15A(0.6) H15B(0.6) H15C(0.6) C18(0.6) H18A(0.6) H18B(0.6) H18C(0.6)
 C3A(0.6) H3AA(0.6) H3AB(0.6) H3AC(0.6) C4A(0.6) H4AA(0.6) H4AB(0.6) H4AC(0.6)
 N3A(0.6) N1(0.4) C2(0.4) H2A(0.4) H2B(0.4) H2C(0.4) C18A(0.4) H18D(0.4)
 H18E(0.4) H18F(0.4) C15A(0.4) H15D(0.4) H15E(0.4) H15F(0.4) C5A(0.4) H5AA(0.4)
 H5AB(0.4) H5AC(0.4)
4.a Me refined with riding coordinates:
 C1(H1BD,H1BE,H1BF), C1(H1AA,H1AB,H1AC), C2A(H2AA,H2AB,H2AC), C3(H3A,H3B,H3C),
 C4(H4A,H4B,H4C), C5(H5C,H5D,H5E), C6(H6C,H6D,H6E), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C3A(H3AA,H3AB,H3AC), C2(H2A,H2B,H2C),
  C18A(H18D,H18E,H18F), C15A(H15D,H15E,H15F)
4.b Idealised Me refined as rotating group:
 C7(H7C,H7D,H7E), C9(H9C,H9D,H9E), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13C,H13D,H13E), C14(H14C,H14D,H14E), C17(H17A,H17B,
 H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), 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),
 C4A(H4AA,H4AB,H4AC), C8(H8C,H8D,H8E), C5A(H5AA,H5AB,H5AC)
;
_shelx_res_checksum              77644
_olex2_submission_special_instructions 'No special instructions were received'