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_7057820
_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 Gd2 N6 O8), 2(C2 H3 N)'
_chemical_formula_sum            'C144 H150 Gd4 N14 O16'
_chemical_formula_weight         2961.77
_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             2018-08-14
_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                110.362(2)
_cell_angle_beta                 93.259(2)
_cell_angle_gamma                109.829(2)
_cell_formula_units_Z            2
_cell_length_a                   17.2276(10)
_cell_length_b                   20.3466(11)
_cell_length_c                   23.4504(11)
_cell_measurement_reflns_used    9729
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.35
_cell_volume                     7105.4(7)
_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      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0805
_diffrn_reflns_av_unetI/netI     0.0814
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            94556
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.477
_diffrn_reflns_theta_min         2.172
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.907
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0714 before and 0.0551 after correction.
The Ratio of minimum to maximum transmission is 0.7789.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.117
_refine_diff_density_min         -1.247
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1603
_refine_ls_number_reflns         29272
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0868P)^2^+1.2852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18826
_reflns_number_total             29272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj04226h2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7057818--7057820.cif.'
_cod_database_code               7057820
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.818
_shelx_estimated_absorpt_t_min   0.581
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C70-C67
 1.5 with sigma of 0.02
 C70-C69
 1.5 with sigma of 0.02
 C10-C11
 1.5 with sigma of 0.02
 C70-C68
 1.5 with sigma of 0.02
 H16-O16
 0.82 with sigma of 0.02
 C69-C68 \\sim C68-C67
 with sigma of 0.02
3. Rigid bond restraints
 C69, C70, C68
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C69 \\sim C67 \\sim C68: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C70 \\sim C68 \\sim C69 \\sim C67: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C140) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C101) \\sim Ueq,
Uanis(C120) \\sim Ueq, Uanis(C116) \\sim Ueq, Uanis(C114) \\sim Ueq,
Uanis(C115) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N14) \\sim Ueq, Uanis(C144) \\sim Ueq, Uanis(C143) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C29) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C141) \\sim Ueq, Uanis(C142) \\sim Ueq, Uanis(N13) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C30) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C68) = Uanis(C69)
5.a Ternary CH refined with riding coordinates:
 O16(H16)
5.b Aromatic/amide H refined with riding coordinates:
 C104(H104), C135(H135), C94(H94), C3(H3), C83(H83), C41(H41), C44(H44),
 C18(H18), C95(H95), C34(H34), C112(H112), C39(H39), C48(H48), C89(H89),
 C72(H72), C110(H110), C7(H7), C8(H8A), C40(H40), C78(H78), C105(H105),
 C19(H19), C111(H111), C24(H24), C79(H79), C42(H42), C2(H2), C46(H46),
 C124(H124), C77(H77), C26(H26), C47(H47), C88(H88), C82(H82), C118(H118),
 C25(H25), C109(H109), C98(H98), C99(H99), C100(H100), C101(H101), C102(H102),
 C54(H54), C35(H35), C93(H93), C96(H96), C28(H28), C29(H29), C30(H30), C31(H31),
  C32(H32), C9(H9), C23(H23), C86(H86), C65(H65), C80(H80), C73(H73),
 C114(H114), C10(H10), C84(H84), C85(H85), C45(H45), C115(H115), C0AA(H0AA),
 C15(H15), C12(H12), C117(H117), C116(H116), C13(H13), C14(H14)
5.c Fitted hexagon refined as free rotating group:
 C97(C98,C99,C100,C101,C102), C27(C28,C29,C30,C31,C32)
5.d Idealised Me refined as rotating group:
 C127(H12A,H12B,H12C), C131(H13A,H13B,H13C), C58(H58A,H58B,H58C), C50(H50A,
 H50B,H50C), C61(H61A,H61B,H61C), C121(H12D,H12E,H12F), C62(H62A,H62B,H62C),
 C128(H12G,H12H,H12I), C129(H12J,H12K,H12L), C132(H13D,H13E,H13F), C51(H51A,
 H51B,H51C), C60(H60A,H60B,H60C), C139(H13G,H13H,H13I), C49(H49A,H49B,H49C),
 C57(H57A,H57B,H57C), C120(H12M,H12N,H12O), C59(H59A,H59B,H59C), C130(H13J,H13K,
 H13L), C119(H11A,H11B,H11C), C138(H13M,H13N,H13O), C67(H67A,H67B,H67C),
 C140(H14A,H14B,H14C), C69(H69A,H69B,H69C), C68(H68A,H68B,H68C), C143(H14D,H14E,
 H14F), C141(H14G,H14H,H14I)
;
_shelx_res_checksum              78073
_shelx_hkl_checksum              31750
_shelx_fab_checksum              16548
_olex2_submission_special_instructions 'No special instructions were received'