Fine-tuning the type of equatorial donor atom in pentagonal bipyramidal Dy(III) complexes to enhance single-molecule magnet properties
Wu, Haipeng; Li, Min; Yin, Bing; Xia, Zhengqiang; Ke, Hongshan; Wei, Qing; Xie, Gang; Chen, Sanping; Gao, Sheng-li; Dalton Transactions  (2019) –; doi:10.1039/C9DT03292D

data_7701292
_publ_section_title
;
 Fine-tuning the type of equatorial donor atom in pentagonal bipyramidal
 Dy(III) complexes to enhance single-molecule magnet properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03292D
_journal_year                    2019
_chemical_formula_moiety         '3(C32 H24 Cl6 Dy N7 O9)'
_chemical_formula_sum            'C96 H72 Cl18 Dy3 N21 O27'
_chemical_formula_weight         3077.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-16 deposited with the CCDC.    2019-10-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.3870(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.3141(7)
_cell_length_b                   18.7255(6)
_cell_length_c                   26.6532(7)
_cell_measurement_reflns_used    9485
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.288
_cell_measurement_theta_min      3.624
_cell_volume                     11635.7(6)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            113380
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.404
_diffrn_reflns_theta_min         2.306
_exptl_absorpt_coefficient_mu    2.401
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.2519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1318 before and 0.0761 after correction. The Ratio of minimum to maximum transmission is 0.3345. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_description       block
_exptl_crystal_F_000             6060
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         5.664
_refine_diff_density_min         -2.719
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1462
_refine_ls_number_reflns         23705
_refine_ls_number_restraints     1599
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0765
_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^)+(0.0920P)^2^+153.2637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1927
_refine_ls_wR_factor_ref         0.2120
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18799
_reflns_number_total             23705
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03292d2.cif
_cod_data_source_block           3
_cod_database_code               7701292
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.762
_shelx_estimated_absorpt_t_min   0.672
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 N9-C38
 1.38 with sigma of 0.02
 C40-N10
 1.38 with sigma of 0.02
 H9-H38A
 2 with sigma of 0.02
 H10-H40B
 2.2 with sigma of 0.02
 H10-H41A
 2 with sigma of 0.02
 H17-H72A
 2 with sigma of 0.02
 H17-H73B
 2.2 with sigma of 0.02
3. Rigid bond restraints
 C32, C27, C28, C31, Cl6
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C32 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C56 \\sim C24 \\sim
C57 \\sim C53 \\sim C54 \\sim C55 \\sim C25 \\sim C59 \\sim C58 \\sim C74 \\sim
C69 \\sim C79 \\sim C85 \\sim C78 \\sim C91 \\sim C21 \\sim C26 \\sim C64 \\sim
C96 \\sim C37 \\sim C80 \\sim C72 \\sim C68 \\sim C90 \\sim C81 \\sim C15 \\sim
C46 \\sim C23 \\sim C39 \\sim C63 \\sim C87 \\sim C86 \\sim C82 \\sim C88 \\sim
C84 \\sim C36 \\sim C95 \\sim C33 \\sim C22 \\sim C65 \\sim C5 \\sim C18 \\sim
C62 \\sim C42 \\sim C60 \\sim C89 \\sim C43 \\sim C83 \\sim C47 \\sim C77 \\sim
C94 \\sim C38 \\sim C35 \\sim C34 \\sim C75 \\sim C19 \\sim C6 \\sim C20 \\sim
C92 \\sim C45 \\sim C61 \\sim C67 \\sim C93 \\sim C41 \\sim C3 \\sim C16 \\sim
C4 \\sim C17 \\sim C70 \\sim C76 \\sim C71 \\sim C50 \\sim C66 \\sim C7 \\sim
C52 \\sim C73 \\sim C1 \\sim C9 \\sim C8 \\sim C44 \\sim C2 \\sim C48 \\sim C40
\\sim C51 \\sim C49 \\sim C10 \\sim C14 \\sim C13 \\sim C12 \\sim C11: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq,
Uanis(N9) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C32) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.001
5.a Ternary CH refined with riding coordinates:
 N16(H16), N9(H9), N2(H2), N17(H17), N10(H10), N3(H3A)
5.b Secondary CH2 refined with riding coordinates:
 C72(H72A,H72B), C39(H39A,H39B), C38(H38A,H38B), C6(H6A,H6B), C41(H41A,H41B),
 C70(H70A,H70B), C71(H71A,H71B), C7(H7A,H7B), C73(H73A,H73B), C9(H9A,H9B),
 C8(H8A,H8B), C40(H40A,H40B)
5.c Aromatic/amide H refined with riding coordinates:
 C29(H29), C31(H31), C57(H57), C55(H55), C25(H25), C78(H78), C68(H68),
 C81(H81), C46(H46), C23(H23), C63(H63), C87(H87), C36(H36), C95(H95), C33(H33),
  C65(H65), C89(H89), C43(H43), C83(H83), C77(H77), C35(H35), C34(H34),
 C75(H75), C19(H19), C45(H45), C61(H61), C67(H67), C93(H93), C3(H3), C4(H4),
 C17(H17A), C76(H76), C66(H66), C1(H1), C44(H44), C2(H2A), C51(H51), C49(H49),
 C14(H14), C13(H13), C12(H12), C11(H11)
5.d Fitted hexagon refined as free rotating group:
 C32(C27,C28,C29,C30,C31), C10(N4,C14,C13,C12,C11)
;
_shelx_res_checksum              66497
_shelx_fab_checksum              39948
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'