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_7246047
_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         'C76 H84 Dy6 N6 O32'
_chemical_formula_sum            'C82 H84 Dy6 N6 O32'
_chemical_formula_weight         2652.64
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-30
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.6360(3)
_cell_length_b                   16.7245(2)
_cell_length_c                   23.9473(3)
_cell_measurement_reflns_used    7957
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3.352
_cell_volume                     9065.9(2)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293.00
_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_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33738
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.352
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    4.966
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_description       block
_exptl_crystal_F_000             5128
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_exptl_transmission_factor_max   0.355
_exptl_transmission_factor_min   0.301
_refine_diff_density_max         2.148
_refine_diff_density_min         -1.395
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         7957
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0305P)^2^+73.5618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6722
_reflns_number_total             7957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01201d2.cif
_cod_data_source_block           lwq-12_auto
_cod_depositor_comments
'Adding full bibliography for 7246045--7246048.cif.'
_cod_database_code               7246047
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.408
_shelx_estimated_absorpt_t_min   0.370
_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, H8 of O8
2. Restrained distances
 C36-C35
 1.5 with sigma of 0.001
 C33-C34
 1.5 with sigma of 0.001
 H13_$1-H33B
 2.2 with sigma of 0.001
 H35A-H11_$2
 2.2 with sigma of 0.001
 H35C-H27_$3
 2.5 with sigma of 0.001
 H1-H2
 2 with sigma of 0.001
3. Rigid bond restraints
 C36, C35
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C34, C33
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4.a Ternary CH refined with riding coordinates:
 O8(H8), O7(H7), N1(H1), N3(H3), C9(H9), C15(H15)
4.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C23(H23A,H23B)
4.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C12(H12), C11(H11), C19(H19), C25(H25), C27(H27), C17(H17), C13(H13),
 C18(H18), C26(H26), C5(H5), C14(H14), C3(H3A), C4(H4)
4.d Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C31(H31A,H31B,H31C), C22(H22A,H22B,
 H22C), C30(H30A,H30B,H30C), C1(H1A,H1B,H1C), C37(H37A,H37B,H37C), C39(H39A,
 H39B,H39C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 280 electrons were 
found in a volume of 1488\%A^3^ in 1 void per unit cell.
 This is consistent with the presence of 
4[CH3OH] per Asymmetric Unit 
which account for 288 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              76204
_shelx_fab_checksum              33731
_olex2_submission_special_instructions 'No special instructions were received'