Two types of Ln<sub>2</sub>Cu<sub>2</sub> hydroxo-trimethylacetate complexes with 0D and 1D motifs: synthetic features, structural differences, and slow magnetic relaxation.
Bovkunova, Anna A.; Bazhina, Evgeniya S.; Evstifeev, Igor S.; Nelyubina, Yulia V.; Shmelev, Maxim A.; Babeshkin, Konstantin A.; Efimov, Nikolay N.; Kiskin, Mikhail A.; Eremenko, Igor L.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 12275–12286; doi:10.1039/d1dt01161h

data_7707995
_publ_section_title
;
 Two types of Ln<sub>2</sub>Cu<sub>2</sub> hydroxo-trimethylacetate
 complexes with 0D and 1D motifs: synthetic features, structural
 differences, and slow magnetic relaxation.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12275
_journal_page_last               12286
_journal_paper_doi               10.1039/d1dt01161h
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C27 H52 Cu Na O12 Tb, C2 H6 O'
_chemical_formula_sum            'C29 H58 Cu Na O13 Tb'
_chemical_formula_weight         860.20
_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   mixed
_audit_creation_date             2021-07-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-16 deposited with the CCDC.	2021-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                111.418(5)
_cell_angle_beta                 92.764(4)
_cell_angle_gamma                109.635(4)
_cell_formula_units_Z            2
_cell_length_a                   11.6772(16)
_cell_length_b                   13.2658(16)
_cell_length_c                   14.5526(19)
_cell_measurement_reflns_used    4099
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.61
_cell_measurement_theta_min      2.19
_cell_volume                     1938.7(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_unetI/netI     0.0770
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16892
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.188
_exptl_absorpt_coefficient_mu    2.423
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0613 before and 0.0470 after correction.
The Ratio of minimum to maximum transmission is 0.7983.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       block
_exptl_crystal_F_000             882
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.276
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         7305
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0321P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6068
_reflns_number_total             7305
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01161h2.cif
_cod_data_source_block           2_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7707992--7707995.cif.'
_cod_database_code               7707995
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.849
_shelx_estimated_absorpt_t_min   0.713
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O13B-C28B = O13A-C28A
 1.35 with sigma of 0.02
 C14-C15B \\sim C14-C17B \\sim C14-C16B \\sim C14-C15A \\sim C14-C17A \\sim
C14-C16A \\sim C14-C13
 with sigma of 0.02
 C15B-C17B \\sim C15B-C16B \\sim C17B-C16B \\sim C15A-C17A \\sim C15A-C16A
\\sim C17A-C16A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C17B) = Uanis(C16B)
Uanis(C15B) = Uanis(C17B)
4. Others
 Sof(O13B)=Sof(H)=Sof(C28B)=Sof(HA)=Sof(HB)=Sof(HC)=Sof(HD)=Sof(HE)=1-FVAR(1)
 Sof(HF)=Sof(HG)=Sof(HH)=Sof(O13A)=Sof(HI)=Sof(C28A)=Sof(HJ)=Sof(HK)=FVAR(1)
 Sof(C15B)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C17B)=Sof(H17A)=Sof(H17B)=
 Sof(H17C)=Sof(C16B)=Sof(H16A)=Sof(H16B)=Sof(H16C)=1-FVAR(2)
 Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=
 Sof(H17F)=Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=FVAR(2)
5.a Riding coordinates:
 O10(H10), O13B(H), O13A(HI)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C28B(HA,HB), C28A(HJ,HK)
5.c Me refined with riding coordinates:
 C17A(H17D,H17E,H17F), C16A(H16D,H16E,H16F)
5.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C4(H4A,H4B,H4C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C), C20(H20A,H20B,H20C), C25(H25A,H25B,H25C), C3(H3A,H3B,H3C), C27(H27A,
 H27B,H27C), C5(H5A,H5B,H5C), C12(H12A,H12B,H12C), C21(H21A,H21B,H21C), C7(H7A,
 H7B,H7C), C22(H22A,H22B,H22C), C29B(HC,HD,HE), C29B(HF,HG,HH), C15B(H15A,H15B,
 H15C), C17B(H17A,H17B,H17C), C16B(H16A,H16B,H16C), C15A(H15D,H15E,H15F)
5.e Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              12750
_shelx_hkl_checksum              71508
_olex2_submission_special_instructions 'No special instructions were received'