Synthesis, luminescence and magnetic properties of tetranuclear lanthanide-based (Eu4, Gd4 and Dy4) clusters
Zhang, Ya-Xin; Zhang, Yue-Hua; Liu, Bi-Ying; Wang, Wen-Min; Tang, Gong-Ping; Wei, Hai-Ying; Wu, Zhi-Lei; New Journal of Chemistry 42 (2018) 18305–; doi:10.1039/C8NJ04226H

data_7057819
_publ_section_title
;
 Synthesis, luminescence and magnetic properties of tetranuclear
 lanthanide-based (Eu4, Gd4 and Dy4) clusters
;
_journal_issue                   22
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18305
_journal_paper_doi               10.1039/C8NJ04226H
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         '2(C70 H72 Eu2 N6 O8), C2 H3 N'
_chemical_formula_sum            'C142 H147 Eu4 N13 O16'
_chemical_formula_weight         2899.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-07-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-14 deposited with the CCDC.
2018-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                110.1633(18)
_cell_angle_beta                 93.286(2)
_cell_angle_gamma                109.9669(17)
_cell_formula_units_Z            2
_cell_length_a                   17.3686(7)
_cell_length_b                   20.3861(8)
_cell_length_c                   23.5088(10)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.23
_cell_volume                     7198.2(5)
_computing_cell_refinement       '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)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1064
_diffrn_reflns_av_unetI/netI     0.0917
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            98142
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.152
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.781
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0740 before and 0.0641 after correction.
The Ratio of minimum to maximum transmission is 0.8514.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       block
_exptl_crystal_F_000             2940
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.103
_refine_diff_density_min         -1.102
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1602
_refine_ls_number_reflns         25357
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1309
_refine_ls_R_factor_gt           0.0729
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+107.5145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16522
_reflns_number_total             25357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj04226h2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7057818--7057820.cif.'
_cod_database_code               7057819
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.655
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O8-H8
 0.82 with sigma of 0.02
 C56A-C57
 2.1 with sigma of 0.02
 H57B-H56D
 2.2 with sigma of 0.02
 H56E-H57B
 2.2 with sigma of 0.02
 O16-H16A
 0.82 with sigma of 0.02
 H56D-H57C
 2.15 with sigma of 0.02
 C56A-C183 \\sim C183-C56B
 with sigma of 0.02
3. Rigid bond restraints
 C57, C58
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C57, C183
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C57 \\sim C58: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N5) \\sim Ueq, Uanis(C183) \\sim Ueq, Uanis(C133) \\sim Ueq, Uanis(C118)
\\sim Ueq, Uanis(C120) \\sim Ueq, Uanis(C137) \\sim Ueq, Uanis(C136) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C56B) \\sim Ueq, Uanis(C57) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C37) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C39) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C141) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C56B) = Uanis(C56A)
5. Others
 Sof(C56A)=Sof(H56D)=Sof(H56E)=Sof(H56F)=1-FVAR(1)
 Sof(C56B)=Sof(H56A)=Sof(H56B)=Sof(H56C)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C47(H47), C108(H108), C94(H94), C39(H39), C16(H16), C111(H111),
 C7(H7), C5(H5), C42(H42), C106(H106), C41(H41), C32(H32), C99(H99), C83(H83),
 C25(H25), C79(H79), C110(H110), C9(H9), C84(H84), C3(H3), C85(H85), C70(H70),
 C10(H10), C46(H46), C15(H15), C26(H26), C100(H100), C54(H54), C116(H116),
 C95(H95), C101(H101), C134(H134), C30(H30), C48(H48), C36(H36), C115(H115),
 C123(H123), C92(H92), C31(H31), C23(H23), C102(H102), C64(H64), C2(H2),
 C117(H117), C103(H103), C76(H76), C1(H1), C86(H86), C87(H87), C88(H88),
 C89(H89), C90(H90), C6(H6), C78(H78), C18(H18), C35(H35), C17(H17), C20(H20),
 C74(H74), C21(H21), C72(H72), C71(H71), C104(H104), C73(H73), C19(H19),
 C37(H37), C105(H105), C33(H33), C34(H34)
6.b Fitted hexagon refined as free rotating group:
 C86(C87,C88,C89,C90,C91)
6.c Idealised Me refined as rotating group:
 C128(H12A,H12B,H12C), C130(H13A,H13B,H13C), C58(H58A,H58B,H58C), C49(H49A,
 H49B,H49C), C51(H51A,H51B,H51C), C126(H12D,H12E,H12F), C50(H50A,H50B,H50C),
 C67(H67A,H67B,H67C), C60(H60A,H60B,H60C), C139(H13D,H13E,H13F), C68(H68A,H68B,
 H68C), C69(H69A,H69B,H69C), C59(H59A,H59B,H59C), C131(H13G,H13H,H13I),
 C138(H13J,H13K,H13L), C129(H12G,H12H,H12I), C119(H11A,H11B,H11C), C61(H61A,
 H61B,H61C), C127(H12J,H12K,H12L), C118(H11D,H11E,H11F), C137(H13M,H13N,H13O),
 C120(H12M,H12N,H12O), C56B(H56A,H56B,H56C), C57(H57A,H57B,H57C), C140(H14A,
 H14B,H14C), C56A(H56D,H56E,H56F)
;
_shelx_res_checksum              80728
_shelx_hkl_checksum              230
_shelx_fab_checksum              19637
_olex2_submission_special_instructions 'No special instructions were received'