Exploiting complementary ligands for the construction of square antiprismatic monometallic lanthanide SMMs.
Jiao, Yushu; Sarwar, Sidra; Sanz, Sergio; van Leusen, Jan; Izarova, Natalya V.; Campbell, Cameron L.; Brechin, Euan K.; Dalgarno, Scott J.; Kögerler, Paul; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9648–9654; doi:10.1039/d1dt00359c

data_7707706
_publ_section_title
;
 Exploiting complementary ligands for the construction of square
 antiprismatic monometallic lanthanide SMMs.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9648
_journal_page_last               9654
_journal_paper_doi               10.1039/d1dt00359c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C56 H72 O8 Tb, C16 H36 N, 0.5(C4 H6 N2)'
_chemical_formula_sum            'C74 H111 N2 O8 Tb'
_chemical_formula_weight         1315.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-03-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.01.31 svn.r88ba2a32 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-12-16 deposited with the CCDC.	2021-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 120.3400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.8191(5)
_cell_length_b                   16.0761(4)
_cell_length_c                   21.0672(5)
_cell_measurement_reflns_used    9496
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.45
_cell_measurement_theta_min      3.49
_cell_volume                     6962.2(3)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'Apex III (Bruker)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            143474
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.686
_diffrn_reflns_theta_min         3.490
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.412
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1017 before and 0.0544 after correction.
The Ratio of minimum to maximum transmission is 0.6824.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.359
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         7092
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.387
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+76.6075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.1399
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7005
_reflns_number_total             7092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00359c2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7707703--7707706.cif.'
_cod_database_code               7707706
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.357
_shelx_estimated_absorpt_t_min   0.190
_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
 C20-C15 = C21-C15 = C19-C15 = C18-C15 = C16-C15 = C17-C15 = C23-C22 = C24-C22
 = C25-C22 = C26-C22 = C27-C22 = C28-C22
 1.54 with sigma of 0.02
 C28-C24
 2.54 with sigma of 0.04
 C25-C27
 2.54 with sigma of 0.04
 C16-C18
 2.54 with sigma of 0.04
 C27-C23
 2.54 with sigma of 0.04
 C18-C20
 2.54 with sigma of 0.04
 C26-C28
 2.54 with sigma of 0.04
 C20-C16
 2.54 with sigma of 0.04
 C24-C26
 2.54 with sigma of 0.04
 C21-C17
 2.54 with sigma of 0.04
 C23-C25
 2.54 with sigma of 0.04
 C17-C19
 2.54 with sigma of 0.04
 C19-C21
 2.54 with sigma of 0.04
3. Others
 Fixed Sof: C16(0.5) H16A(0.5) H16B(0.5) H16C(0.5) C18(0.5) H18A(0.5)
 H18B(0.5) H18C(0.5) C20(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C23(0.5) H23A(0.5)
 H23B(0.5) H23C(0.5) C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5) C27(0.5) H27A(0.5)
 H27B(0.5) H27C(0.5) C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C19(0.5) H19A(0.5)
 H19B(0.5) H19C(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C24(0.5) H24A(0.5)
 H24B(0.5) H24C(0.5) C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5) C28(0.5) H28A(0.5)
 H28B(0.5) H28C(0.5) H43A(0.5) H43B(0.5) H43C(0.5) N1(0.5) C44(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
 C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C9(H9), C11(H11), C32(H32)
4.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C16(H16A,H16B,
 H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C25(H25A,
 H25B,H25C), C27(H27A,H27B,H27C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C),
 C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C28(H28A,H28B,
 H28C), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              77088
_shelx_hkl_checksum              27266
_olex2_submission_special_instructions 'No special instructions were received'