Magnetic investigation in di- and tetranuclear lanthanide complexes
Wu, Jianfeng; Liu, Dan; Yang, Qianqian; Ge, Yan; Tang, Jinkui; Qi, Zhenhui; New Journal of Chemistry 45 (2021) 2200–2207; doi:10.1039/D0NJ04247A

data_7060173
_publ_section_title
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 Magnetic investigation in di- and tetranuclear lanthanide complexes
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2200
_journal_page_last               2207
_journal_paper_doi               10.1039/D0NJ04247A
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C56 H60 Dy2 N8 O17 S4, 2(C2 N), C2 H3 N'
_chemical_formula_sum            'C62 H69 Dy2 N11 O17 S4'
_chemical_formula_weight         1693.52
_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     dual
_audit_creation_date             2020-06-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
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2020-06-11 deposited with the CCDC.	2020-12-18 downloaded from the CCDC.
;
_cell_angle_alpha                85.497(3)
_cell_angle_beta                 79.190(3)
_cell_angle_gamma                75.155(3)
_cell_formula_units_Z            2
_cell_length_a                   13.8109(8)
_cell_length_b                   14.5458(8)
_cell_length_c                   18.5543(10)
_cell_measurement_reflns_used    9597
_cell_measurement_temperature    180
_cell_measurement_theta_max      62.356
_cell_measurement_theta_min      2.425
_cell_volume                     3537.2(3)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      180.0
_diffrn_measured_fraction_theta_full 0.854
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0815
_diffrn_reflns_av_unetI/netI     0.0820
_diffrn_reflns_Laue_measured_fraction_full 0.854
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33743
_diffrn_reflns_point_group_measured_fraction_full 0.854
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         62.434
_diffrn_reflns_theta_min         2.425
_exptl_absorpt_coefficient_mu    12.890
_exptl_absorpt_correction_T_max  0.191
_exptl_absorpt_correction_T_min  0.145
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       block
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.111
_refine_diff_density_min         -1.643
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     918
_refine_ls_number_reflns         10945
_refine_ls_number_restraints     1319
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1183
_refine_ls_R_factor_gt           0.0976
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+83.8110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2168
_refine_ls_wR_factor_ref         0.2307
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8773
_reflns_number_total             10945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04247a2.cif
_cod_data_source_block           Dy2
_cod_depositor_comments
'Adding full bibliography for 7060172--7060173.cif.'
_cod_database_code               7060173
_shelxl_version_number           2013-4
_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) groups, All O(H,H) groups
2. Restrained distances
 N11-C62
 1.12 with sigma of 0.01
 N10-C60
 1.12 with sigma of 0.01
 N9-C58
 1.12 with sigma of 0.01
 C62-C63
 1.46 with sigma of 0.02
 C60-C61
 1.46 with sigma of 0.02
 C58-C59
 1.46 with sigma of 0.02
 N9-C59
 2.6 with sigma of 0.02
 N10-C61
 2.6 with sigma of 0.02
 N11-C63
 2.6 with sigma of 0.02
 C6AA-C5AA
 2.28 with sigma of 0.02
 C2AA-C3AA
 2.2 with sigma of 0.02
 O2-H2
 0.87 with sigma of 0.01
 O5-H5
 0.87 with sigma of 0.01
 C1-H2
 1.908453 with sigma of 0.02
 Dy1-H2
 3.016966 with sigma of 0.02
 C29-H5
 1.872183 with sigma of 0.02
 Dy2-H5
 3.040822 with sigma of 0.02
 Dy1-N0AA \\sim Dy1-N2AB
 with sigma of 0.02
 N0AA-C1AA \\sim N2AB-N1AB
 with sigma of 0.02
 N0AA-N1AA \\sim N2AB-C3AB
 with sigma of 0.02
 C1AA-C0AA \\sim N1AB-C0AA
 with sigma of 0.02
 C1AA-C6AA \\sim N1AB-C6AA
 with sigma of 0.02
 N1AA-C8AA \\sim C3AB-C8AA
 with sigma of 0.02
 N1AA-C5AA \\sim C3AB-C5AA
 with sigma of 0.02
 Dy1-C1AA \\sim Dy1-N1AB
 with sigma of 0.04
 Dy1-N1AA \\sim Dy1-C3AB
 with sigma of 0.04
 N0AA-C8AA \\sim N2AB-C8AA
 with sigma of 0.04
 N0AA-C0AA \\sim N2AB-C0AA
 with sigma of 0.04
 N0AA-C6AA \\sim N2AB-C6AA
 with sigma of 0.04
 N0AA-C5AA \\sim N2AB-C5AA
 with sigma of 0.04
 C1AA-N1AA \\sim N1AB-C3AB
 with sigma of 0.04
 Dy2-N3AA \\sim Dy2-N3AB
 with sigma of 0.02
 C20-C7AA \\sim C20-N7AB
 with sigma of 0.02
 C24-N2AA \\sim C24-C4AA
 with sigma of 0.02
 N3AA-N2AA \\sim N3AB-C4AA
 with sigma of 0.02
 N3AA-C7AA \\sim N3AB-N7AB
 with sigma of 0.02
 N2AA-C2AA \\sim C4AA-C2AA
 with sigma of 0.02
 C7AA-C3AA \\sim N7AB-C3AA
 with sigma of 0.02
 Dy2-N2AA \\sim Dy2-C4AA
 with sigma of 0.04
 Dy2-C7AA \\sim Dy2-N7AB
 with sigma of 0.04
 C20-N3AA \\sim C20-N3AB
 with sigma of 0.04
 C24-N3AA \\sim C24-N3AB
 with sigma of 0.04
 N3AA-C2AA \\sim N3AB-C2AA
 with sigma of 0.04
 N3AA-C3AA \\sim N3AB-C3AA
 with sigma of 0.04
 N2AA-C7AA \\sim C4AA-N7AB
 with sigma of 0.04
3. Rigid bond restraints
 C61, C60
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C59, C58
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C24) \\sim Ueq,
Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(C29) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C59) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(N11)
\\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(N9) \\sim Ueq, Uanis(N10) \\sim Ueq,
Uanis(C60) \\sim Ueq, Uanis(C63) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C61) = Uanis(C60)
Uanis(C59) = Uanis(C58)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C6AA)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(N1AB)=Sof(N2AB)=Sof(C3AB)=
 Sof(H3AB)=Sof(C3AA)=Sof(H3AA)=Sof(H3AC)=Sof(H3AD)=Sof(C4AA)=Sof(H4AA)=
 Sof(N3AB)=Sof(N7AB)=1-FVAR(1)
 Sof(N0AA)=Sof(C1AA)=Sof(H1AA)=Sof(N1AA)=Sof(C5AA)=Sof(H5AA)=Sof(H5AB)=
 Sof(H5AC)=Sof(N3AA)=Sof(N2AA)=Sof(C7AA)=Sof(H7AA)=Sof(C2AA)=Sof(H2AA)=
 Sof(H2AB)=Sof(H2AC)=FVAR(1)
7.a Rotating group:
 O1(H1A,H1B)
7.b Secondary CH2 refined with riding coordinates:
 C1(H1C,H1D), C14(H14A,H14B), C15(H15A,H15B), C29(H29A,H29B)
7.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C19(H19), C3(H3), C4(H4), C5(H5A), C10(H10), C11(H11),
 C12(H12), C25(H25), C26(H26), C27(H27), C32(H32), C33(H33), C35(H35), C36(H36),
  C39(H39), C40(H40), C42(H42), C43(H43), C46(H46), C47(H47), C49(H49),
 C50(H50), C53(H53), C54(H54), C56(H56), C57(H57), C1AA(H1AA), C3AB(H3AB),
 C7AA(H7AA), C4AA(H4AA)
7.d Fitted hexagon refined as free rotating group:
 N5(C16,C17,C18,C19,C20), C28(N8,C24,C25,C26,C27)
7.e Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C37(H37A,H37B,H37C), C44(H44A,H44B,H44C), C51(H51A,H51B,
 H51C), C63(H63A,H63B,H63C), C6AA(H6AA,H6AB,H6AC), C5AA(H5AA,H5AB,H5AC),
 C2AA(H2AA,H2AB,H2AC), C3AA(H3AA,H3AC,H3AD)
;
_shelx_res_checksum              44972
_olex2_submission_special_instructions 'No special instructions were received'