Understanding a pentagonal-bipyramidal holmium(iii) complex with a record energy barrier for magnetisation reversal.
Ma, Yan; Zhai, Yuan-Qi; Ding, You-Song; Han, Tian; Zheng, Yan-Zhen; Chemical communications (Cambridge, England) 56 (2020) 3979–3982; doi:10.1039/d0cc00500b

data_7126087
_publ_section_title
;
 Understanding a pentagonal-bipyramidal holmium(iii) complex with a record
 energy barrier for magnetisation reversal.
;
_journal_issue                   28
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3979
_journal_page_last               3982
_journal_paper_doi               10.1039/d0cc00500b
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety
'C41 H43 Ho N5 O2, C24 H20 B, 1.5(C5 H5 N), 0.5(C5 H6 N)'
_chemical_formula_sum            'C75 H73.5 B Ho N7 O2'
_chemical_formula_weight         1280.64
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-11-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-01 deposited with the CCDC.	2020-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                101.047(9)
_cell_angle_beta                 93.207(9)
_cell_angle_gamma                90.009(9)
_cell_formula_units_Z            4
_cell_length_a                   15.645(11)
_cell_length_b                   15.651(11)
_cell_length_c                   28.55(2)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      25.60
_cell_measurement_theta_min      2.33
_cell_volume                     6850(8)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            68037
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.875
_diffrn_reflns_theta_min         1.304
_exptl_absorpt_coefficient_mu    1.204
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       block
_exptl_crystal_F_000             2642
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.28
_exptl_transmission_factor_max   0.714
_exptl_transmission_factor_min   0.655
_refine_diff_density_max         2.065
_refine_diff_density_min         -3.037
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1557
_refine_ls_number_reflns         25855
_refine_ls_number_restraints     176
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+40.1245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1625
_refine_ls_wR_factor_ref         0.1713
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20379
_reflns_number_total             25855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00500b2.cif
_cod_data_source_block           1_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7126084--7126087.cif.'
_cod_original_cell_volume        6851(8)
_cod_original_formula_sum        'C75 H73.50 B Ho N7 O2'
_cod_database_code               7126087
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.729
_shelx_estimated_absorpt_t_min   0.671
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C7AA-C6AA
 1.37 with sigma of 0.01
 C7AA-C8AA
 1.37 with sigma of 0.01
 C8AA-C9AA
 1.37 with sigma of 0.01
 C9AA-N0BA
 1.35 with sigma of 0.01
 N0BA-C1BA
 1.35 with sigma of 0.01
 C1BA-C6AA
 1.37 with sigma of 0.01
 C7AA-N0BA
 2.67 with sigma of 0.01
 C1BA-C8AA
 2.67 with sigma of 0.01
 C6AA-C9AA
 2.77 with sigma of 0.02
3. Rigid bond restraints
 C28, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C30, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C18, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C21B, C22B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C24B, C25B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C0AA \\sim C2AA \\sim C3AA \\sim N4AA \\sim N4AA \\sim C5AA \\sim C5AA \\sim
C2AA: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
C38 \\sim C36: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C39 \\sim C38: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C17) \\sim Ueq, Uanis(C22B) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C23B)
\\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C24B) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C70) \\sim Ueq, Uanis(C3AA) \\sim Ueq, Uanis(N4AA) \\sim Ueq, Uanis(C5AA)
\\sim Ueq, Uanis(C7AA) \\sim Ueq, Uanis(C6AA) \\sim Ueq, Uanis(C9AA) \\sim Ueq,
Uanis(N0BA) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C2AA)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C40B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C38) \\sim Ueq, Uanis(C3B) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.001
5.a Secondary CH2 refined with riding coordinates:
 C2AA(H2AA,H2AB)
5.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C35(H35), C33(H33), C27B(H27B), C30(H30), C59B(H59B), C33B(H33B),
 C5B(H5B), C38(H38), C35B(H35B), C30B(H30B), C38B(H38B), C11(H11), C15B(H15B),
 C6B(H6B), C15(H15), C24(H24), C27(H27), C12(H12), C9B(H9B), C65(H65),
 C11B(H11B), C47B(H47B), C65B(H65B), C1B(H1B), C17B(H17B), C16B(H16B),
 C41B(H41B), C46B(H46B), C10B(H10B), C25(H25), C1(H1), C49B(H49B), C12B(H12B),
 C43B(H43B), C20B(H20B), C14B(H14B), C8B(H8B), C23(H23), C64(H64), C14(H14),
 C10(H10), C21(H21), C13B(H13B), C7B(H7B), C4B(H4B), C58B(H58B), C18B(H18B),
 C19B(H19B), C55B(H55B), C61(H61), C61B(H61B), C64B(H64B), C56B(H56B),
 C57B(H57B), C9(H9), C53(H53), C63(H63), C2B(H2B), C6(H6), C59(H59), C13(H13),
 C55(H55), C50B(H50B), C53B(H53B), C63B(H63B), C57(H57), C47(H47), C5(H5),
 C45B(H45B), C44B(H44B), C3B(H3B), C22(H22), C62B(H62B), C2(H2), C49(H49),
 C20(H20), C7(H7), C8(H8), C3(H3), C43(H43), C4(H4), C16(H16), C62(H62),
 C51B(H51B), C58(H58), C66B(H66B), C25B(H25B), C56(H56), C52B(H52B), C52(H52),
 C67B(H67B), C21B(H21B), C51(H51), C68B(H68B), C44(H44), C46(H46), C17(H17),
 C50(H50), C22B(H22B), C70B(H70B), C19(H19), C24B(H24B), C69B(H69B), C45(H45),
 C18(H18), C70(H70), C23B(H23B), C69(H69), C66(H66), C67(H67), C68(H68),
 C0AA(H0AA), C3AA(H3AA), C1AA(H1AA), C5AA(H5AA), C1BA(H1BA), C9AA(H9AA),
 C7AA(H7AA), C6AA(H6AA), C8AA(H8AA)
5.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C29B(H29D,H29E,H29F), C32B(H32D,H32E,H32F), C37(H37A,
 H37B,H37C), C29(H29A,H29B,H29C), C37B(H37D,H37E,H37F), C40B(H40D,H40E,H40F),
 C32(H32A,H32B,H32C)
;
_shelx_res_checksum              90783
_olex2_submission_special_instructions 'No special instructions were received'