Synthesis, structures and magnetic properties of four dysprosium-based complexes with a multidentate ligand with steric constraint
Li, Wen-Qiang; Ma, Meng-Xia; Ni, Qing-Ling; Li, Shi-Ming; Gui, Liu-Cheng; Wang, Xiu-Jian; CrystEngComm 25 (2023) 614–621; doi:10.1039/D2CE01201D

data_7246045
_publ_section_title
;
 Synthesis, structures and magnetic properties of four dysprosium-based
 complexes with a multidentate ligand with steric constraint
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              614
_journal_page_last               621
_journal_paper_doi               10.1039/D2CE01201D
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C46 H56 Dy5 N3 O24'
_chemical_formula_sum            'C46 H56 Dy5 N3 O24'
_chemical_formula_weight         1850.46
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-08-29
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-11-15 deposited with the CCDC.	2022-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.1370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.98250(10)
_cell_length_b                   22.9575(2)
_cell_length_c                   23.0079(2)
_cell_measurement_reflns_used    10115
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.601
_cell_measurement_theta_min      2.733
_cell_volume                     5742.60(9)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Image Plate'
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44427
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         2.733
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    34.862
_exptl_absorpt_correction_T_max  0.002
_exptl_absorpt_correction_T_min  0.002
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.140
_exptl_crystal_description       block
_exptl_crystal_F_000             3512
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.672
_refine_diff_density_min         -1.900
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         10115
_refine_ls_number_restraints     269
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0550P)^2^+64.5754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9269
_reflns_number_total             10115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01201d2.cif
_cod_data_source_block           20220709-wxj-lwq-dy5_auto
_cod_depositor_comments
'Adding full bibliography for 7246045--7246048.cif.'
_cod_database_code               7246045
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.062
_shelx_estimated_absorpt_t_min   0.051
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H1-H2
 2.1 with sigma of 0.01
3. Rigid bond restraints
 C7, C6, C29, C24, C23, C36, C40, C9, C46, C32, C5, C15, C33, C38, C34, C47,
 C44, C28, C22, C42, C4, C39, C13, C14, C11, C8, C10, C45, C3, C1, C37, C25,
 C41, C27, C26, C30, C31, C43, C18, C17, C16, C21, C20, C19, C12, C35
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C7 \\sim C6 \\sim C29 \\sim C24 \\sim C23 \\sim C36 \\sim C40 \\sim C9 \\sim
C46 \\sim C32 \\sim C5 \\sim C15 \\sim C33 \\sim C38 \\sim C34 \\sim C47 \\sim
C44 \\sim C28 \\sim C22 \\sim C42 \\sim C4 \\sim C39 \\sim C13 \\sim C14 \\sim
C11 \\sim C8 \\sim C10 \\sim C45 \\sim C3 \\sim C1 \\sim C37 \\sim C25 \\sim
C41 \\sim C27 \\sim C26 \\sim C30 \\sim C31 \\sim C43 \\sim C18 \\sim C17 \\sim
C16 \\sim C21 \\sim C20 \\sim C19 \\sim C12 \\sim C35: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01 within 2A
5.a Ternary CH refined with riding coordinates:
 N1(H1), N3(H3), C9(H9), C15(H15), O8(H8a)
5.b Secondary CH2 refined with riding coordinates:
 C23(H23a,H23b), C46(H46a,H46b)
5.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), N2(H2), C13(H13), C14(H14), C11(H11), C8(H8), C3(H3a),
 C25(H25), C27(H27), C26(H26), C18(H18), C17(H17), C19(H19)
5.d Fitted hexagon refined as free rotating group:
 N2(C13,C14,C11,C8,C10), C18(C17,C16,C21,C20,C19)
5.e Idealised Me refined as rotating group:
 C33(H33a,H33b,H33c), C22(H22a,H22b,H22c), C39(H39a,H39b,H39c), C45(H45a,H45b,
 H45c), C1(H1a,H1b,H1c), C37(H37a,H37b,H37c), C41(H41a,H41b,H41c), C30(H30a,
 H30b,H30c), C31(H31a,H31b,H31c), C43(H43a,H43b,H43c), C12(H12a,H12b,H12c),
 C35(H35a,H35b,H35c)
;
_olex2_submission_special_instructions 'No special instructions were received'