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_7057818
_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 Dy2 N6 O8), 2(C2 H3 N)'
_chemical_formula_sum            'C144 H150 Dy4 N14 O16'
_chemical_formula_weight         2982.77
_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                110.327(2)
_cell_angle_beta                 93.328(2)
_cell_angle_gamma                109.820(2)
_cell_formula_units_Z            2
_cell_length_a                   17.1171(8)
_cell_length_b                   20.3908(10)
_cell_length_c                   23.5026(12)
_cell_measurement_reflns_used    9820
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.34
_cell_volume                     7091.4(6)
_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 0.992
_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  0.1005
_diffrn_reflns_av_unetI/netI     0.0812
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_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       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            109179
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.441
_diffrn_reflns_theta_min         2.092
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.147
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0823 before and 0.0618 after correction.
The Ratio of minimum to maximum transmission is 0.7952.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       block
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.611
_refine_diff_density_min         -1.328
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1633
_refine_ls_number_reflns         26067
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0864P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17111
_reflns_number_total             26067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj04226h2.cif
_cod_data_source_block           mo_3
_cod_depositor_comments
'Adding full bibliography for 7057818--7057820.cif.'
_cod_database_code               7057818
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.798
_shelx_estimated_absorpt_t_min   0.575
_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
 C7-C6
 1.42 with sigma of 0.02
 O8-H8
 0.82 with sigma of 0.02
3. Rigid bond restraints
 C78, C79, C77
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C21, C22, C17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C78 \\sim C79 \\sim C76 \\sim C77: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C78) \\sim Ueq, Uanis(C77) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C21) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N0AA) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C1AA) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C138) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Ternary CH refined with riding coordinates:
 O16(H16)
5.b Aromatic/amide H refined with riding coordinates:
 C135(H135), C116(H116), C101(H101), C25(H25), C42(H42), C117(H117), C31(H31),
 C62(H62), C112(H112), C111(H111), C106(H106), C26(H26), C10(H10), C39(H39),
 C55(H55), C46(H46), C23(H23), C100(H100), C57(H57), C49(H49), C107(H107),
 C47(H47), C52(H52), C81(H81), C124(H124), C63(H63), C64(H64), C87(H87),
 C96(H96), C53(H53), C41(H41), C95(H95), C102(H102), C9(H9), C58(H58),
 C2AA(H2AA), C70(H70), C109(H109), C33(H33), C93(H93), C51(H51), C32(H32),
 C90(H90), C91(H91), C7(H7), C14(H14), C104(H104), C30(H30), C37(H37), C89(H89),
  C88(H88), C15(H15), C118(H118), C103(H103), C105(H105), C34(H34), C1(H1),
 C5(H5), C2(H2), C3(H3), C4(H4), C48(H48), C35(H35), C36(H36), C20(H20),
 C17(H17), C21(H21), C19(H19), C18(H18), C50(H50)
5.c Idealised Me refined as rotating group:
 C131(H13A,H13B,H13C), C65(H65A,H65B,H65C), C141(H14D,H14E,H14F), C127(H12A,
 H12B,H12C), C73(H73A,H73B,H73C), C130(H13D,H13E,H13F), C120(H12D,H12E,H12F),
 C66(H66A,H66B,H66C), C121(H12G,H12H,H12I), C84(H84A,H84B,H84C), C132(H13G,H13H,
 H13I), C85(H85A,H85B,H85C), C139(H13J,H13K,H13L), C76(H76A,H76B,H76C),
 C86(H86A,H86B,H86C), C140(H14A,H14B,H14C), C74(H74A,H74B,H74C), C67(H67A,H67B,
 H67C), C75(H75A,H75B,H75C), C138(H13M,H13N,H13O), C78(H78A,H78B,H78C),
 C77(H77A,H77B,H77C), C129(H12J,H12K,H12L), C128(H12M,H12N,H12O), C119(H11A,
 H11B,H11C), C1AA(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              70472
_shelx_hkl_checksum              826
_shelx_fab_checksum              53496
_olex2_submission_special_instructions 'No special instructions were received'