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_7707992
_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 Dy Na O12, C2 H6 O'
_chemical_formula_sum            'C29 H58 Cu Dy Na O13'
_chemical_formula_weight         863.78
_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             2021-03-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-03-25 deposited with the CCDC.	2021-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                111.336(4)
_cell_angle_beta                 92.570(4)
_cell_angle_gamma                110.320(3)
_cell_formula_units_Z            2
_cell_length_a                   11.8623(11)
_cell_length_b                   13.4002(13)
_cell_length_c                   14.7222(18)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      30.21
_cell_measurement_theta_min      2.16
_cell_volume                     2004.5(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'three-circle diffractometer'
_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  0.0192
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            62544
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.625
_exptl_absorpt_coefficient_mu    2.443
_exptl_absorpt_correction_T_max  0.3812
_exptl_absorpt_correction_T_min  0.2758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0719 before and 0.0370 after correction. The Ratio of minimum to maximum transmission is 0.7235. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       prism
_exptl_crystal_F_000             884
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         7757
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0092P)^2^+4.0763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0592
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7263
_reflns_number_total             7757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01161h2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7707992--7707995.cif.'
_cod_database_code               7707992
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.641
_shelx_estimated_absorpt_t_min   0.580
_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 O(H) groups
2. Restrained distances
 C15A-C16A \\sim C15A-C14A \\sim C16A-C14A \\sim C14-C16 \\sim C16-C15
 with sigma of 0.04
 C13B-C13 \\sim C13B-C15A \\sim C13B-C16A \\sim C13B-C14A \\sim C13B-C14 \\sim
C13B-C16 \\sim C13B-C15
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C24) = Uanis(C24A)
Uanis(C25) = Uanis(C25A)
Uanis(C18) = Uanis(C21)
Uanis(C2) = Uanis(C3A)
Uanis(C20) = Uanis(C19A)
4. Others
 Sof(C24)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C26)=Sof(H26D)=Sof(H26E)=Sof(H26F)=
 Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C25)=Sof(H25A)=Sof(H25B)=
 Sof(H25C)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(1)
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=1-FVAR(2)
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(2)
 Sof(C21)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C19)=Sof(H19D)=Sof(H19E)=Sof(H19F)=
 Sof(C20)=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(3)
 Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21A)=Sof(H21A)=Sof(H21B)=
 Sof(H21C)=Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(3)
 Sof(O13A)=Sof(H13A)=Sof(C28)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C27)=Sof(H27C)=
 Sof(H27D)=1-FVAR(4)
 Sof(O13)=Sof(H13)=Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(C28A)=Sof(H28A)=Sof(H28B)=
 Sof(H28C)=FVAR(4)
 Sof(C14)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C16)=Sof(H16D)=Sof(H16E)=Sof(H16F)=
 Sof(C15)=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(5)
 Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16A)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(5)
5.a Riding coordinates:
 C14(H14D,H14E,H14F), C15(H15D,H15E,H15F)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C27A(H27A,H27B), C27(H27C,H27D)
5.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C7(H7A,H7B,
 H7C), C26A(H26A,H26B,H26C), C25(H25A,H25B,H25C), C24A(H24A,H24B,H24C),
 C24(H24D,H24E,H24F), C26(H26D,H26E,H26F), C25A(H25D,H25E,H25F), C4(H4A,H4B,
 H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,
 H5AC), C3A(H3AA,H3AB,H3AC), C20A(H20A,H20B,H20C), C21A(H21A,H21B,H21C),
 C19A(H19A,H19B,H19C), C21(H21D,H21E,H21F), C19(H19D,H19E,H19F), C20(H20D,H20E,
 H20F), C28A(H28A,H28B,H28C), C28(H28D,H28E,H28F), C15A(H15A,H15B,H15C),
 C16A(H16A,H16B,H16C), C14A(H14A,H14B,H14C), C16(H16D,H16E,H16F)
5.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O13(H13), O13A(H13A)
;
_shelx_res_checksum              79655
_shelx_hkl_checksum              94772
_olex2_submission_special_instructions 'No special instructions were received'