Interplay between anisotropy and magnetic exchange to modulate magnetic relaxation behaviors of phenoxo bridged Dy2 dimers with axial β-diketonate co-ligands
Roy, Soumalya; Shukla, Pooja; Ahmed, Naushad; Du, Ming-Hao; Tarannum, Ibtesham; Kong, Xiang-Jian; Gupta, Tulika; Singh, Saurabh Kumar Kumar; Das, Sourav; Dalton Transactions  (2022) –; doi:10.1039/D2DT03117E

data_7711748
_publ_section_title
;
 Interplay between anisotropy and magnetic exchange to modulate magnetic
 relaxation behaviors of phenoxo bridged Dy2 dimers with axial
 \b-diketonate co-ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT03117E
_journal_year                    2022
_chemical_formula_moiety         'C57 H75 Dy2 N5 O11'
_chemical_formula_sum            'C57 H75 Dy2 N5 O11'
_chemical_formula_weight         1331.22
_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     iterative
_audit_creation_date             2022-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-11-06 deposited with the CCDC.	2022-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.401(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2636(18)
_cell_length_b                   35.219(5)
_cell_length_c                   13.709(2)
_cell_measurement_reflns_used    9046
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.29
_cell_volume                     6350.5(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            57384
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         2.320
_exptl_absorpt_coefficient_mu    2.391
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1122 before and 0.0622 after correction. The Ratio of minimum to maximum transmission is 0.5431. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.046
_exptl_crystal_size_mid          0.037
_exptl_crystal_size_min          0.024
_refine_diff_density_max         1.972
_refine_diff_density_min         -1.749
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         11725
_refine_ls_number_restraints     244
_refine_ls_restrained_S_all      1.221
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0571
_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^)+(0.0001P)^2^+59.0393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1250
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10877
_reflns_number_total             11725
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03117e2.cif
_cod_data_source_block           Compound_03
_cod_original_cell_volume        6350.7(16)
_cod_database_code               7711748
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C50-C48
 1.52 with sigma of 0.02
 C50-C47
 1.52 with sigma of 0.02
3. Rigid bond restraints
 C48, C50, C49, C47
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C56, C57, C54, C55, C53, C52, C51, C50, C48, C47, C49
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C36, C38, C37, C39, C41, C42, C43, C46, C44, C45, C40
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C37, C36, C39, C38
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C50 \\sim C47 \\sim C48 \\sim C49: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04
C53 \\sim C54 \\sim C57 \\sim C55 \\sim C56 \\sim C52 \\sim C51 \\sim C50 \\sim
C47 \\sim C48 \\sim C49: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim
C46 \\sim C44 \\sim C45: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C36 \\sim C37 \\sim C39 \\sim C38: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C50) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C48)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C49)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C38)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C56) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C55)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C56) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C55)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C50) = Uanis(C48) = Uanis(C49) = Uanis(C47)
5.a Aromatic/amide H refined with riding coordinates:
 C30(H30), C19(H19), C2(H2), C5(H5), C14(H14), C17(H17), C16(H16), C7(H7),
 C24(H24), C21(H21), C41(H41), C3(H3), C22(H22), C15(H15), C9(H9), C4(H4),
 C12(H12), C23(H23), C11(H11), C10(H10), C52(H52)
5.b Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C25(H25A,H25B,H25C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C57(H57A,H57B,H57C), C55(H55A,
 H55B,H55C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C45(H45A,H45B,H45C),
 C39(H39A,H39B,H39C), C56(H56A,H56B,H56C), C36(H36A,H36B,H36C), C38(H38A,H38B,
 H38C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              17570
_shelx_fab_checksum              90453
_olex2_submission_special_instructions 'No special instructions were received'