Structures, fluorescence properties and magnetic properties of a series of rhombus-shaped LnIII4 clusters: magnetocaloric effect and single-molecule-magnet behavior
Wang, Wen-Min; Zhang, Li; Li, Xian-Zhen; He, Li-Yuan; Wang, Xin-Xin; Shi, Ying; Wang, Jie; Dong, Jie; Wu, Zhi-Lei; New Journal of Chemistry 43 (2019) 12941–; doi:10.1039/C9NJ02872B

data_7058613
_publ_section_title
;
 Structures, fluorescence properties and magnetic properties of a series
 of rhombus-shaped LnIII4 clusters: magnetocaloric effect and
 single-molecule-magnet behavior
;
_journal_issue                   33
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12941
_journal_paper_doi               10.1039/C9NJ02872B
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         '2(C64 H60 Ho2 N6 O8), C2 H3 N, C2 H6 O'
_chemical_formula_sum            'C132 H129 Ho4 N13 O17'
_chemical_formula_weight         2829.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-06-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-01 deposited with the CCDC.    2019-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                67.850(12)
_cell_angle_beta                 71.409(11)
_cell_angle_gamma                64.294(9)
_cell_formula_units_Z            2
_cell_length_a                   17.7355(18)
_cell_length_b                   19.8419(16)
_cell_length_c                   20.6173(18)
_cell_measurement_reflns_used    14581
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     5949.1(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            76055
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.552
_diffrn_reflns_theta_min         3.032
_exptl_absorpt_coefficient_mu    2.703
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.757
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1534
_refine_ls_number_reflns         26823
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+9.4559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.1095
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19785
_reflns_number_total             26823
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02872b2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7058609--7058615.cif.'
_cod_original_cell_volume        5949.1(12)
_cod_database_code               7058613
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.737
_shelx_estimated_absorpt_t_min   0.614
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H8 of O8, H16 of O16, All C(H,H) groups, All C(H,H,H,H)
  groups
 At 1.5 times of:
  All C(H,H,H) groups, H1AA of O1AA
2. Restrained distances
 C81-C82 = C81-C82' = C99-C100 = C99-C10'
 1.54 with sigma of 0.01
 H12B-H13B
 2.2 with sigma of 0.02
 H0AA-H36A
 2.2 with sigma of 0.02
 H36C-H0AC
 2.2 with sigma of 0.02
 H36A-H0AC
 2.2 with sigma of 0.02
 C0AA-O1AA
 2.9 with sigma of 0.02
 H1AA_$1-H10F_$2
 2.2 with sigma of 0.02
 C2AA-O1AA
 1.1 with sigma of 0.02
 H1AA-H10D_$3
 2.2 with sigma of 0.02
3. Rigid bond restraints
 N13, C129, C130
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C82 \\sim C82': within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C100 \\sim C10': within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C130 \\sim C129 \\sim N13: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C121) \\sim Ueq, Uanis(C122) \\sim Ueq, Uanis(C123) \\sim Ueq,
Uanis(C130) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C82) \\sim Ueq, Uanis(C82') \\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C10')
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N13) \\sim Ueq, Uanis(C129) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C2AA) \\sim Ueq, Uanis(O1AA) \\sim Ueq, Uanis(C0AA) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(H81C)=Sof(H81D)=Sof(C82')=Sof(H82D)=Sof(H82E)=Sof(H82F)=1-FVAR(1)
 Sof(H81A)=Sof(H81B)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=FVAR(1)
 Sof(H99C)=Sof(H99D)=Sof(C10')=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(2)
 Sof(H99A)=Sof(H99B)=Sof(C100)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 O8(H8), O16(H16)
6.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C35(H35A,H35B), C53(H53A,H53B), C81(H81A,H81B), C81(H81C,
 H81D), C99(H99A,H99B), C99(H99C,H99D), C117(H11A,H11B), C2AA(H2AA,H2AB)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8A), C9(H9), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16A), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27),
 C28(H28), C30(H30), C31(H31), C33(H33), C34(H34), C39(H39), C40(H40), C43(H43),
  C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C51(H51), C52(H52),
 C57(H57), C62(H62), C67(H67), C68(H68), C71(H71), C72(H72), C73(H73), C74(H74),
  C76(H76), C77(H77), C79(H79), C80(H80), C85(H85), C86(H86), C89(H89),
 C90(H90), C91(H91), C92(H92), C94(H94), C95(H95), C97(H97), C98(H98),
 C103(H103), C104(H104), C107(H107), C108(H108), C109(H109), C110(H110),
 C112(H112), C113(H113), C115(H115), C116(H116), C121(H121), C126(H126)
6.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C36(H36A,H36B,H36C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C64(H64A,H64B,H64C), C82(H82A,
 H82B,H82C), C82'(H82D,H82E,H82F), C100(H10A,H10B,H10C), C10'(H10D,H10E,H10F),
 C118(H11C,H11D,H11E), C119(H11F,H11G,H11H), C123(H12A,H12B,H12C), C124(H12D,
 H12E,H12F), C128(H12G,H12H,H12I), C130(H13A,H13B,H13C), C0AA(H0AA,H0AB,H0AC)
6.e Idealised tetrahedral OH refined as rotating group:
 O1AA(H1AA)
;
_shelx_res_checksum              39873
_olex2_submission_special_instructions 'No special instructions were received'