Role of molecular symmetry in the magnetic relaxation dynamics of five-coordinate Dy(III) complexes.
Guo, Yan; Liu, Kang; Qin, Yuanyuan; Wu, Qunyan; Hu, Kongqiu; Mei, Lei; Chai, Zhifang; Liu, Xiangyu; Yu, Jipan; Shi, Weiqun; Dalton transactions (Cambridge, England : 2003) 52 (2023) 2703–2711; doi:10.1039/d3dt00095h

data_7712479
_publ_section_title
;
 Role of molecular symmetry in the magnetic relaxation dynamics of
 five-coordinate Dy(III) complexes.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2703
_journal_page_last               2711
_journal_paper_doi               10.1039/d3dt00095h
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C34 H53 Dy N4 O Si3'
_chemical_formula_sum            'C34 H53 Dy N4 O Si3'
_chemical_formula_weight         780.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-10-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-10-16 deposited with the CCDC.	2023-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.790(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0282(5)
_cell_length_b                   19.3323(9)
_cell_length_c                   19.4044(10)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      2.38
_cell_volume                     3682.5(3)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            76565
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_min         1.503
_exptl_absorpt_coefficient_mu    2.158
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       block
_exptl_crystal_F_000             1604
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.124(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     825
_refine_ls_number_reflns         16866
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0265
_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^)+(0.0110P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0456
_refine_ls_wR_factor_ref         0.0473
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                15394
_reflns_number_total             16866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00095h2.cif
_cod_data_source_block           mo_yu1_0m
_cod_database_code               7712479
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.876(5)
 0.124(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C51) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C69)
\\sim Ueq, Uanis(C50) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=
 Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=1-FVAR(1)
 Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=
 Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C59(H59A,H59B), C22(H22A,H22B), C15(H15A,H15B), C14(H14A,H14B), C58(H58A,
 H58B), C4(H4A,H4B), C39(H39A,H39B), C35(H35A,H35B), C1(H1A,H1B), C38(H38A,
 H38B), C36(H36A,H36B), C37(H37A,H37B), C2(H2A,H2B), C3(H3A,H3B)
5.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C64(H64), C10(H10), C25(H25), C17(H17), C62(H62), C20(H20), C12(H12),
 C19(H19), C63(H63), C11(H11), C18(H18), C61(H61), C27(H27), C41(H41), C26(H26),
  C54(H54), C53(H53), C43(H43), C28(H28), C44(H44), C56(H56), C42(H42), C55(H55)
5.c Idealised Me refined as rotating group:
 C67(H67A,H67B,H67C), C48(H48A,H48B,H48C), C33(H33A,H33B,H33C), C5(H5A,H5B,
 H5C), C34(H34A,H34B,H34C), C30(H30A,H30B,H30C), C47(H47A,H47B,H47C), C66(H66A,
 H66B,H66C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C29(H29A,H29B,H29C), C68(H68A,
 H68B,H68C), C31(H31A,H31B,H31C), C46(H46A,H46B,H46C), C32(H32A,H32B,H32C),
 C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C50(H50A,H50B,H50C), C69(H69A,H69B,
 H69C), C71(H71A,H71B,H71C), C70(H70A,H70B,H70C)
;
_shelx_res_checksum              93016
_shelx_hkl_checksum              28222
_olex2_submission_special_instructions 'No special instructions were received'