Engineering macrocyclic high performance pentagonal bipyramidal Dy(iii) single-ion magnets.
Canaj, Angelos B.; Dey, Sourav; Wilson, Claire; Céspedes, Oscar; Rajaraman, Gopalan; Murrie, Mark; Chemical communications (Cambridge, England) 56 (2020) 12037–12040; doi:10.1039/d0cc04559d

data_7127164
_publ_section_title
;
 Engineering macrocyclic high performance pentagonal bipyramidal Dy(iii)
 single-ion magnets.
;
_journal_issue                   80
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12037
_journal_page_last               12040
_journal_paper_doi               10.1039/d0cc04559d
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C53 H57 Dy N5 O2 Si2, C H2 Cl2, C24 H20 B'
_chemical_formula_sum            'C78 H79 B Cl2 Dy N5 O2 Si2'
_chemical_formula_weight         1418.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-06-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-30 deposited with the CCDC.	2020-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                100.425(3)
_cell_angle_beta                 103.832(3)
_cell_angle_gamma                100.857(3)
_cell_formula_units_Z            4
_cell_length_a                   14.3753(11)
_cell_length_b                   22.1443(17)
_cell_length_c                   23.4355(19)
_cell_measurement_reflns_used    9782
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.974
_cell_measurement_theta_min      2.209
_cell_volume                     6911.6(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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150
_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  '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  0.0400
_diffrn_reflns_av_unetI/netI     0.0471
_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       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            103339
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.892
_diffrn_reflns_theta_min         2.209
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.244
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1182 before and 0.0511 after correction. The Ratio of minimum to maximum transmission is 0.8657. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       block
_exptl_crystal_F_000             2924
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         5.190
_refine_diff_density_min         -1.911
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1644
_refine_ls_number_reflns         32846
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0682
_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^)+(0.1007P)^2^+21.5032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1824
_refine_ls_wR_factor_ref         0.1988
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24960
_reflns_number_total             32846
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04559d2.cif
_cod_data_source_block           mo_at_1055_sec_0m
_cod_depositor_comments          'Adding full bibliography for 7127164.cif.'
_cod_original_cell_volume        6911.6(9)
_cod_database_code               7127164
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.896
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups,
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C41A-C42A
 1.5 with sigma of 0.02
 C42A-C41A
 1.51 with sigma of 0.02
 N5A-C53A \\sim N5A-C54A \\sim N4A-C50A \\sim N4A1-C50A \\sim N4A-C49A \\sim
N4A1-C49A \\sim N3A1-C46A
 \\sim N3A-C46A \\sim N3A1-C48A \\sim N3A-C47A
 with sigma of 0.01
 C54A-C51A \\sim C52A-C53A \\sim C51A-C50A \\sim C50A-C52A \\sim C49A-C47A
\\sim C49A-C48A
 with sigma of 0.02
 N4B-C48B \\sim N4B-C47B \\sim N3B-C49B \\sim N3B1-C50B \\sim N3B1-C51B \\sim
N3B-C51B
 with sigma of 0.01
 C46B-C45B \\sim C45B-C47B \\sim C45B-C44B \\sim C49B-C48B \\sim C48B-C50B
\\sim C51B-C52B \\sim C53B-
 C51B \\sim C54B-C52B \\sim C54B-C53B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C48A \\sim C47A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N4A1 \\sim N4A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C52A \\sim C51A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C54A \\sim C53A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N3A1 \\sim N3A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C57A \\sim C56A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
4. Others
 Fixed Sof: H46A(0.6) H46B(0.6) H46C(0.4) H46D(0.4) H49A(0.6) H49B(0.6)
 H49C(0.4) H49D(0.4) H50A(0.6) H50B(0.6) H50C(0.4) H50D(0.4) N3A(0.6) H3AA(0.6)
 N4A(0.6) H4AA(0.6) C47A(0.6) H47A(0.6) H47B(0.6) C51A(0.6) H51A(0.6) H51B(0.6)
 C54A(0.6) H54A(0.6) H54B(0.6) C56A(0.4) H56A(0.4) H56B(0.4) H56C(0.4)
 N3A1(0.4) H3A1(0.4) N4A1(0.4) H4A1(0.4) C48A(0.4) H48A(0.4) H48B(0.4)
 C53A(0.4) H53A(0.4) H53B(0.4) C52A(0.4) H52A(0.4) H52B(0.4) C57A(0.6)
 H57A(0.6) H57B(0.6) H57C(0.6) H4B(0.5) H4BA(0.5) H45C(0.5) H45D(0.5) H45E(0.5)
 H45F(0.5) H48C(0.5) H48D(0.5) H48E(0.5) H48F(0.5) H51C(0.5) H51D(0.5)
 H51E(0.5) H51F(0.5) H54C(0.5) H54D(0.5) H54E(0.5) H54F(0.5) N3B(0.5) H3BA(0.5)
 C46B(0.5) H46E(0.5) H46F(0.5) C49B(0.5) H49E(0.5) H49F(0.5) C53B(0.5)
 H53C(0.5) H53D(0.5) N3B1(0.5) H3B1(0.5) C50B(0.5) H50E(0.5) H50F(0.5)
 C47B(0.5) H47C(0.5) H47D(0.5) C52B(0.5) H52C(0.5) H52D(0.5)
5.a Ternary CH refined with riding coordinates:
 N3A(H3AA), N4A(H4AA), N3A1(H3A1), N4A1(H4A1), N4B(H4B), N4B(H4BA), N3B(H3BA),
 N3B1(H3B1)
5.b Secondary CH2 refined with riding coordinates:
 C44A(H44A,H44B), C45A(H45A,H45B), C46A(H46A,H46B), C46A(H46C,H46D), C49A(H49A,
 H49B), C49A(H49C,H49D), C50A(H50A,H50B), C50A(H50C,H50D), C47A(H47A,H47B),
 C51A(H51A,H51B), C54A(H54A,H54B), C48A(H48A,H48B), C53A(H53A,H53B), C52A(H52A,
 H52B), C44B(H44C,H44D), C45B(H45C,H45D), C45B(H45E,H45F), C48B(H48C,H48D),
 C48B(H48E,H48F), C51B(H51C,H51D), C51B(H51E,H51F), C54B(H54C,H54D), C54B(H54E,
 H54F), C46B(H46E,H46F), C49B(H49E,H49F), C53B(H53C,H53D), C50B(H50E,H50F),
 C47B(H47C,H47D), C52B(H52C,H52D), C1S(H1SA,H1SB), C2S(H2SA,H2SB)
5.c Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A), C8A(H8A), C9A(H9A),
 C10A(H10A), C11A(H11A), C12A(H12A), C14A(H14A), C15A(H15A), C16A(H16A),
 C17A(H17A), C18A(H18A), C20A(H20A), C21A(H21A), C22A(H22A), C23A(H23A),
 C24A(H24A), C26A(H26A), C27A(H27A), C28A(H28A), C29A(H29A), C30A(H30A),
 C32A(H32A), C33A(H33A), C34A(H34A), C35A(H35A), C36A(H36A), C38A(H38A),
 C39A(H39A), C40A(H40A), C2B(H2B), C3B(H3B), C4B(H4BB), C5B(H5B), C6B(H6B),
 C8B(H8B), C9B(H9B), C10B(H10B), C11B(H11B), C12B(H12B), C14B(H14B), C15B(H15B),
  C16B(H16B), C17B(H17B), C18B(H18B), C20B(H20B), C21B(H21B), C22B(H22B),
 C23B(H23B), C24B(H24B), C26B(H26B), C27B(H27B), C28B(H28B), C29B(H29B),
 C30B(H30B), C32B(H32B), C33B(H33B), C34B(H34B), C35B(H35B), C36B(H36B),
 C39B(H39B), C40B(H40B), C38B(H38B), C2C(H2C), C3C(H3C), C4C(H4C), C5C(H5C),
 C6C(H6C), C9C(H9C), C10C(H10C), C11C(H11C), C12C(H12C), C13C(H13C), C14C(H14C),
  C15C(H15C), C16C(H16C), C17C(H17C), C18C(H18C), C21C(H21C), C22C(H22C),
 C23C(H23C), C24C(H24C), C25C(H25C), C27C(H27C), C28C(H28C), C29C(H29C),
 C30C(H30C), C31C(H31C), C33C(H33C), C34C(H34C), C35C(H35C), C36C(H36C),
 C37C(H37C), C39C(H39C), C40C(H40C), C41C(H41C), C42C(H42C), C43C(H43G),
 C45C(H45G), C46C(H46G), C47C(H47E), C48C(H48G), C49C(H49G)
5.d Idealised Me refined as rotating group:
 C43A(H43A,H43B,H43C), C56A(H56A,H56B,H56C), C57A(H57A,H57B,H57C), C43B(H43D,
 H43E,H43F), C56B(H56D,H56E,H56F)
;
_shelx_res_checksum              22694
_shelx_hkl_checksum              26364
_olex2_submission_special_instructions 'No special instructions were received'