A mononuclear nine-coordinated Dy(iii) complex exhibiting field-induced single-ion magnetism behaviour
Hu, Biao; Xi, Jing; Cen, Peipei; Guo, Yan; Ding, Yi; Qin, Yuanyuan; Zhang, Yi-Quan; Liu, Xiangyu; RSC Advances 12 (2022) 13992–13998; doi:10.1039/D2RA02260E

data_7244910
_publ_section_title
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 A mononuclear nine-coordinated Dy(iii) complex exhibiting field-induced
 single-ion magnetism behaviour
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_journal_issue                   22
_journal_name_full               'RSC Advances'
_journal_page_first              13992
_journal_page_last               13998
_journal_paper_doi               10.1039/D2RA02260E
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C27 H24 Dy N15 O3, 2(H2 O)'
_chemical_formula_sum            'C27 H28 Dy N15 O5'
_chemical_formula_weight         805.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-02-23 deposited with the CCDC.	2022-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.5920(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8382(14)
_cell_length_b                   9.3932(8)
_cell_length_c                   21.5579(18)
_cell_measurement_reflns_used    4898
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.095
_cell_measurement_theta_min      2.603
_cell_volume                     3148.0(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15595
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.007
_diffrn_reflns_theta_max         25.007
_diffrn_reflns_theta_min         1.316
_exptl_absorpt_coefficient_mu    2.438
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.0693 before and 0.0492 after correction.
The Ratio of minimum to maximum transmission is 0.8919.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_description       block
_exptl_crystal_F_000             1604
_refine_diff_density_max         1.679
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.402
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         5523
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+2.4668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.1029
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4112
_reflns_number_total             5523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra02260e2.cif
_cod_data_source_block           x22
_cod_database_code               7244910
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H1WA-O1W
 0.82 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C27) \\sim Ueq, Uanis(N15) \\sim Ueq, Uanis(N15A) \\sim Ueq, Uanis(C27A)
\\sim Ueq, Uanis(N10A) \\sim Ueq, Uanis(N10) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C18A) \\sim Ueq, Uanis(N10A) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(N10)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(N15) \\sim Ueq, Uanis(N15A) \\sim Ueq,
Uanis(C27A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N10) = Uanis(N10A)
Uanis(C18) = Uanis(C18A)
4. Others
 Fixed Sof: H26A(0.5) H26B(0.5) H26C(0.5) H26D(0.5) H17A(0.5) H17B(0.5)
 H17C(0.5) H17D(0.5) C18A(0.5) N10A(0.5) C18(0.5) N10(0.5) C27(0.5) N15(0.5)
 N15A(0.5) C27A(0.5)
5.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
5.b Rotating group:
 N12(H12A,H12B), N2(H2A,H2B)
5.c Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C26(H26C,H26D), C8(H8A,H8B), C17(H17A,H17B), C17(H17C,H17D)
5.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C22(H22), C13(H13), C1(H1), C12(H12), C19(H19), C21(H21),
 C20(H20), C4(H4), C2(H2), C3(H3)
5.e X=CH2 refined with riding coordinates:
 N7(H7A,H7B)
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_shelx_res_checksum              83044
_olex2_submission_special_instructions 'No special instructions were received'