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_7126086
_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
'C31 H43 Ho N5 O2 Si2, C24 H20 B, C2 H2 N, 2(C5 H5 N)'
_chemical_formula_sum            'C67 H75 B Ho N8 O2 Si2'
_chemical_formula_weight         1256.27
_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             2019-08-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-31 deposited with the CCDC.	2020-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                95.521(2)
_cell_angle_beta                 108.465(2)
_cell_angle_gamma                90.850(2)
_cell_formula_units_Z            2
_cell_length_a                   13.665(2)
_cell_length_b                   14.335(2)
_cell_length_c                   17.329(3)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.74
_cell_measurement_theta_min      2.74
_cell_volume                     3201.2(9)
_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
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.975
_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  0.0230
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29507
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.782
_diffrn_reflns_theta_min         1.573
_exptl_absorpt_coefficient_mu    1.322
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       block
_exptl_crystal_F_000             1298
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.745
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         13311
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+3.3339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12017
_reflns_number_total             13311
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00500b2.cif
_cod_data_source_block           1_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7126084--7126087.cif.'
_cod_database_code               7126086
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.778
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C63-N8 = C67-N8
 1.32 with sigma of 0.01
 C63-C64 = C64-C65 = C65-C66 = C66-C67
 1.36 with sigma of 0.01
 C63-C64
 1.36 with sigma of 0.01
3. Rigid bond restraints
 C63, C64, C65, C66, C67
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(N8) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C65)
\\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C63) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C16(H16), C21(H21), C43(H43), C15(H15), C17(H17), C11(H11), C39(H39),
 C20(H20), C10(H10), C31(H31), C14(H14), C12(H12), C45(H45), C26(H26), C30(H30),
  C42(H42), C22(H22), C46(H46), C40(H40), C18(H18), C19(H19), C49(H49),
 C13(H13), C52(H52), C33(H33), C47(H47), C41(H41), C25(H25), C8(H8), C9(H9),
 C55(H55), C53(H53), C37(H37), C51(H51), C29(H29), C27(H27), C54(H54), C56(H56),
  C62(H62), C48(H48), C57(H57), C61(H61), C24(H24), C23(H23), C36(H36),
 C34(H34), C35(H35), C58(H58), C28(H28), C60(H60), C59(H59), C63(H63), C64(H64),
  C66(H66), C67(H67), C65(H65)
5.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C4(H4A,
 H4B,H4C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              17380
_olex2_submission_special_instructions 'No special instructions were received'