Slow magnetic relaxation and selective luminescent probe in a 2p–3d–4f heterotrispin chain
Zhu, Mei; Ma, Shuqi; Dong, Huiyang; Zhong, Qing; Liu, Yi; CrystEngComm 25 (2023) 403–416; doi:10.1039/D2CE01200F

data_7245930
_publ_section_title
;
 Slow magnetic relaxation and selective luminescent probe in a 2p--3d--4f
 heterotrispin chain
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              403
_journal_page_last               416
_journal_paper_doi               10.1039/D2CE01200F
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C65 H53 Cu F30 N6 O18 Tb'
_chemical_formula_sum            'C65 H53 Cu F30 N6 O18 Tb'
_chemical_formula_weight         1998.59
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc29gj4g
_audit_creation_date             2019-11-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-12-16 deposited with the CCDC.	2022-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.406(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0730(14)
_cell_length_b                   19.5641(15)
_cell_length_c                   23.334(2)
_cell_measurement_reflns_used    9615
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.03
_cell_measurement_theta_min      2.19
_cell_volume                     8114.8(11)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0902
_diffrn_reflns_av_unetI/netI     0.1063
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            59016
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.503
_diffrn_reflns_theta_min         2.058
_exptl_absorpt_coefficient_mu    1.262
_exptl_absorpt_correction_T_max  0.3334
_exptl_absorpt_correction_T_min  0.2614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1371 before and 0.0618 after correction. The Ratio of minimum to maximum transmission is 0.7840. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_description       needle
_exptl_crystal_F_000             3972
_refine_diff_density_max         1.248
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1100
_refine_ls_number_reflns         18587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1524
_refine_ls_R_factor_gt           0.0700
_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^)+(0.0784P)^2^+14.7617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1622
_refine_ls_wR_factor_ref         0.2042
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9587
_reflns_number_total             18587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01200f2.cif
_cod_data_source_block           Tb
_cod_depositor_comments
'Adding full bibliography for 7245927--7245932.cif.'
_cod_original_cell_volume        8114.7(11)
_cod_database_code               7245930
_shelx_shelxl_version_number     2014/7
_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.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C36(H36A,H36B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C54(H54), C12(H12), C19(H19), C13(H13), C18(H18), C35(H35), C57(H57),
 C32(H32), C56(H56), C44(H44), C31(H31), C33(H33), C17(H17), C39(H39), C49(H49),
  C20(H20), C28(H28), C23(H23)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C62(H62A,H62B,H62C), C6(H6A,H6B,H6C), C1(H1A,H1B,H1C),
 C14(H14A,H14B,H14C), C58(H58A,H58B,H58C), C2(H2A,H2B,H2C), C65(H65A,H65B,H65C),
  C64(H64A,H64B,H64C), C61(H61A,H61B,H61C)
;
_shelx_res_checksum              7548
_shelx_hkl_checksum              7319
_olex2_submission_special_instructions 'No special instructions were received'