Dysprosium(iii) complexes with a square-antiprism configuration featuring mononuclear single-molecule magnetic behaviours based on different β-diketonate ligands and auxiliary ligands.
Zhang, Sheng; Ke, Hongshan; Shi, Quan; Zhang, Jangwei; Yang, Qi; Wei, Qing; Xie, Gang; Wang, Wenyuan; Yang, Desuo; Chen, Sanping; Dalton transactions (Cambridge, England : 2003) 45 (2016) 5310–5320; doi:10.1039/c6dt00219f

data_7038397
_publ_section_title
;
 Dysprosium(iii) complexes with a square-antiprism configuration featuring
 mononuclear single-molecule magnetic behaviours based on different
 \b-diketonate ligands and auxiliary ligands.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5310
_journal_page_last               5320
_journal_paper_doi               10.1039/c6dt00219f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C52 H33 Dy F9 N2 O6'
_chemical_formula_sum            'C52 H33 Dy F9 N2 O6'
_chemical_formula_weight         1115.30
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-28
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-02-09 deposited with the CCDC.
2016-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.438(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.748(6)
_cell_length_b                   10.942(3)
_cell_length_c                   21.315(5)
_cell_measurement_reflns_used    10079
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.242
_cell_measurement_theta_min      0.944
_cell_volume                     5033(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1345
_diffrn_reflns_av_unetI/netI     0.1874
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26282
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.438
_diffrn_reflns_theta_min         0.944
_exptl_absorpt_coefficient_mu    1.567
_exptl_absorpt_correction_T_max  0.731
_exptl_absorpt_correction_T_min  0.575
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
;
_refine_diff_density_max         1.023
_refine_diff_density_min         -1.046
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         10079
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1326P)^2^+89.4697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1741
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6094
_reflns_number_total             10079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00219f2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7038396--7038398.cif.'
_cod_database_code               7038397
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.731
_shelx_estimated_absorpt_t_min   0.575
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C52-C50
 2.5 with sigma of 0.02
 F6-F5
 2.1 with sigma of 0.02
 F4-F5
 2.1 with sigma of 0.02
 F5-F4
 2.4 with sigma of 0.02
 F5-F6
 2.4 with sigma of 0.02
3. Rigid bond restraints
 C40, C41
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C38, C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F5, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C51, C50
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F7, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(F7) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C40)
\\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C6) \\sim Ueq,
Uanis(C21) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq,
Uanis(C49) \\sim Ueq, Uanis(F8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B)
6.b Aromatic/amide H refined with riding coordinates:
 C40(H40), C42(H42), C20(H20), C28(H28), C43(H43), C39(H39), C17(H17),
 C34(H34), C52(H52), C49(H49), C14(H14), C6(H6), C38(H38), C21(H21), C24(H24),
 C11(H11), C7(H7), C25(H25), C23(H23), C45(H45), C12(H12), C35(H35), C46(H46),
 C44(H44), C26(H26), C51(H51), C37(H37), C50(H50), C10(H10), C9(H9), C3(H3)
;