Self-assembly of octanuclear Ln(iii)-based clusters: their large magnetocaloric effects and highly efficient conversion of CO2
Wang, Wen-Min; Xin, Xiao-Yan; Qiao, Na; Wu, Zhi-Lei; Li, Ling; Zou, Ji-Yong; Dalton Transactions  (2022) –; doi:10.1039/D2DT01892F

data_7711090
_publ_section_title
;
 Self-assembly of octanuclear Ln(iii)-based clusters: their large
 magnetocaloric effects and highly efficient conversion of CO2
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01892F
_journal_year                    2022
_chemical_formula_moiety         'C72 H98 Dy8 N6 O32'
_chemical_formula_sum            'C72 H98 Dy8 N6 O32'
_chemical_formula_weight         2859.56
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-07-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-07-27 deposited with the CCDC.	2022-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                101.562(5)
_cell_angle_beta                 103.649(4)
_cell_angle_gamma                115.059(4)
_cell_formula_units_Z            1
_cell_length_a                   12.9500(13)
_cell_length_b                   14.4583(14)
_cell_length_c                   14.5993(14)
_cell_measurement_reflns_used    5496
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.27
_cell_volume                     2261.9(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       '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  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0990
_diffrn_reflns_av_unetI/netI     0.0850
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30719
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.271
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.598
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1133 before and 0.0690 after correction.
The Ratio of minimum to maximum transmission is 0.6790.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.099
_exptl_crystal_description       block
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.272
_refine_diff_density_min         -1.278
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         7806
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0468
_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^)+20.7178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0915
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5255
_reflns_number_total             7806
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01892f2.cif
_cod_data_source_block           2
_cod_database_code               7711090
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.438
_shelx_estimated_absorpt_t_min   0.227
_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
 O16-H16
 0.82 with sigma of 0.02
 O15-H15
 0.82 with sigma of 0.02
 Dy4_$1-H16 \\sim H16-Dy2_$1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C27) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C29) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C30) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C20) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C36(H36A,H36B), C12(H12A,H12B)
4.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C7(H7), C30(H30), C3(H3), C1(H1), C10(H10), C2(H2), C4(H4), C15(H15A),
  C20(H20), C25(H25)
4.c Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C23(H23A,H23B,H23C), C28(H28A,H28B,H28C), C32(H32A,H32B,
 H32C), C17(H17A,H17B,H17C), C27(H27A,H27B,H27C), C13(H13A,H13B,H13C), C33(H33A,
 H33B,H33C), C22(H22A,H22B,H22C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              36830
_shelx_hkl_checksum              22831
_olex2_submission_special_instructions 'No special instructions were received'