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_7246048
_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         'C62 H60 Dy2 N6 O14'
_chemical_formula_sum            'C62 H60 Dy2 N6 O14'
_chemical_formula_weight         1442.19
_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
_atom_sites_solution_primary     iterative
_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                79.139(3)
_cell_angle_beta                 89.186(3)
_cell_angle_gamma                64.683(4)
_cell_formula_units_Z            2
_cell_length_a                   14.1814(5)
_cell_length_b                   15.2007(7)
_cell_length_c                   17.7267(6)
_cell_measurement_reflns_used    8669
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.999
_cell_measurement_theta_min      3.388
_cell_volume                     3382.9(3)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'marXperts MX300 CCD Detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42871
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.388
_exptl_absorpt_coefficient_mu    2.254
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       block
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_transmission_factor_max   0.682
_exptl_transmission_factor_min   0.629
_refine_diff_density_max         3.081
_refine_diff_density_min         -1.409
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         11868
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0067P)^2^+16.3973P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.1062
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8669
_reflns_number_total             11868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01201d2.cif
_cod_data_source_block           Dy2
_cod_depositor_comments
'Adding full bibliography for 7246045--7246048.cif.'
_cod_database_code               7246048
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.701
_shelx_estimated_absorpt_t_min   0.649
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H4-H41
 2.1 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 N1(H1), N3(H3), N6(H6), N4(H4), C9(H9), C15(H15), C45(H45), C39(H39)
3.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C23(H23A,H23B), C38(H38A,H38B), C53(H53A,H53B)
3.c Aromatic/amide H refined with riding coordinates:
 N5(H5), C3(H3A), C4(H4A), C5(H5A), C11(H11), C12(H12), C13(H13), C14(H14),
 C17(H17), C18(H18), C19(H19), C25(H25), C26(H26), C27(H27), C49(H49), C48(H48),
  C47(H47), C41(H41), C42(H42), C43(H43), C44(H44), C33(H33), C34(H34),
 C35(H35), C55(H55), C56(H56), C57(H57)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C22(H22A,H22B,H22C), C30(H30A,H30B,H30C), C52(H52A,H52B,
 H52C), C31(H31A,H31B,H31C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 126 electrons were 
found in a volume of 734\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[2CH3CN], 1[1CH3OH] per Asymmetric Unit 
which account for 128 electrons 
per unit cell.
;
_shelx_res_checksum              95261
_shelx_fab_checksum              8563
_olex2_submission_special_instructions 'No special instructions were received'