The near-infrared luminescence and magnetism of dinuclear complexes with different local symmetries constructed from a β-diketonate co-ligand and bis-Schiff base ligand
Chen, Huan-Huan; Wu, Dong-Fang; Duan, Yao-Yao; Li, Ling; Wang, Yun-Juan; Zhang, Xue-Mei; Cui, Jian-Zhong; Gao, Hong-Ling; New Journal of Chemistry 44 (2020) 2561–2570; doi:10.1039/C9NJ05571A

data_7059214
_publ_section_title
;
 The near-infrared luminescence and magnetism of dinuclear complexes with
 different local symmetries constructed from a \b-diketonate co-ligand and
 bis-Schiff base ligand
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2561
_journal_page_last               2570
_journal_paper_doi               10.1039/C9NJ05571A
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C80 H68 Dy2 N2 O13'
_chemical_formula_sum            'C80 H68 Dy2 N2 O13'
_chemical_formula_weight         1590.36
_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     direct
_audit_creation_date             2019-04-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-06 deposited with the CCDC.	2020-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                80.69(3)
_cell_angle_beta                 83.18(3)
_cell_angle_gamma                68.42(3)
_cell_formula_units_Z            2
_cell_length_a                   13.547(3)
_cell_length_b                   13.789(3)
_cell_length_c                   19.612(4)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.8664
_cell_measurement_theta_min      1.0543
_cell_volume                     3354.8(14)
_computing_cell_refinement       crystalclear
_computing_data_collection       crystalclear
_computing_data_reduction        crystalclear
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Saturn 70 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0751
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39047
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.768
_diffrn_reflns_theta_min         1.801
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.279
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.028
_refine_diff_density_min         -1.882
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     924
_refine_ls_number_reflns         15684
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12204
_reflns_number_total             15684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05571a2.cif
_cod_data_source_block           Dy
_cod_depositor_comments
;Adding full bibliography for 7059214--7059218.cif.

 Adding full bibliography for 7059214--7059218.cif.
;
_cod_original_cell_volume        3354.7(14)
_cod_database_code               7059214
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.772
_shelx_estimated_absorpt_t_min   0.659
_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, All O(H,H) groups
2. Restrained distances
 C80-O13 = C80A-O13
 1.45 with sigma of 0.01
 N1-C9 = N1-C9A = N2-C10 = N2-C10A
 1.5 with sigma of 0.01
 C9-C10 = C9-C11 = C9A-C10A = C9A-C11A
 1.54 with sigma of 0.01
 O13-H13
 0.87 with sigma of 0.01
 O13-H13A
 0.87 with sigma of 0.01
 C80-H13
 1.908787 with sigma of 0.02
 Dy2-H13
 2.939632 with sigma of 0.02
 C80A-H13A
 1.908718 with sigma of 0.02
 Dy2-H13A
 2.913791 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C80A)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C9A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C11A)=Sof(H11D)=Sof(H11E)=
 Sof(H11F)=1-FVAR(1)
 Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C11)=Sof(H11A)=Sof(H11B)=
 Sof(H11C)=FVAR(1)
 Sof(H13A)=Sof(C80A)=Sof(H80D)=Sof(H80E)=Sof(H80F)=1-FVAR(2)
 Sof(H13)=Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(H80C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C9(H9), C9A(H9A)
5.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C10A(H10C,H10D)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C12(H12), C14(H14), C15(H15), C16(H16),
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C27(H27), C30(H30), C31(H31),
  C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
 C39(H39), C42(H42), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50),
  C51(H51), C52(H52), C53(H53), C54(H54), C57(H57), C60(H60), C61(H61),
 C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69),
  C72(H72), C75(H75), C76(H76), C77(H77), C78(H78), C79(H79)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C19(H19A,H19B,H19C), C80(H80A,H80B,H80C), C11(H11A,H11B,
 H11C), C11A(H11D,H11E,H11F), C80A(H80D,H80E,H80F)
;
_shelx_res_checksum              86107
_olex2_submission_special_instructions 'No special instructions were received'