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_7246046
_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         'C60 H64 Cl6 Dy4 N6 O14'
_chemical_formula_sum            'C60 H60 Cl6 Dy4 N6 O14'
_chemical_formula_weight         1953.85
_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   geom
_audit_creation_date             2022-08-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-11-15 deposited with the CCDC.	2022-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                96.322(3)
_cell_angle_beta                 98.838(2)
_cell_angle_gamma                111.745(3)
_cell_formula_units_Z            1
_cell_length_a                   10.9250(3)
_cell_length_b                   11.2522(4)
_cell_length_c                   16.2537(5)
_cell_measurement_reflns_used    7361
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.371
_cell_measurement_theta_min      3.313
_cell_volume                     1803.23(11)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'marXperts MX300 CCD Detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0483
_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       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25793
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.313
_exptl_absorpt_coefficient_mu    4.379
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_description       block
_exptl_crystal_F_000             942
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   0.455
_exptl_transmission_factor_min   0.333
_refine_diff_density_max         1.360
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         7361
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0231P)^2^+0.0674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0658
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5815
_reflns_number_total             7361
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01201d2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7246045--7246048.cif.'
_cod_database_code               7246046
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.506
_shelx_estimated_absorpt_t_min   0.396
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H7 of O7, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H4 of O4
2.a Ternary CH refined with riding coordinates:
 O7(H7), N1(H1), N3(H3), C9(H9), C15(H15)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C23(H23A,H23B)
2.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C14(H14), C27(H27), C25(H25), C11(H11), C18(H18), C12(H12),
 C26(H26), C19(H19), C3(H3A), C13(H13), C5(H5), C4(H4A)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C30(H30A,H30B,H30C), C22(H22A,H22B,H22C)
2.e Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 70 electrons were 
found in a volume of 306\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[CH3OH] per Asymmetric Unit 
which account for 72 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              48935
_shelx_fab_checksum              12134
_olex2_submission_special_instructions 'No special instructions were received'