A stable dysprosium(iii) complex with a terminal fluoride ligand showing high resolution luminescence and slow magnetic relaxation.
Ling, Bo-Kai; Zhai, Yuan-Qi; Han, Junbo; Han, Tian; Zheng, Yan-Zhen; Dalton transactions (Cambridge, England : 2003) 49 (2020) 6969–6973; doi:10.1039/d0dt01146k

data_7704487
_publ_section_title
;
 A stable dysprosium(iii) complex with a terminal fluoride ligand showing
 high resolution luminescence and slow magnetic relaxation.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6969
_journal_page_last               6973
_journal_paper_doi               10.1039/d0dt01146k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C20 H36 Dy F O8, 4(C H6 N3), 2(C5 H9 O2)'
_chemical_formula_sum            'C34 H78 Dy F N12 O12'
_chemical_formula_weight         1028.58
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-04-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-23 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.934(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.676(9)
_cell_length_b                   13.168(7)
_cell_length_c                   22.406(12)
_cell_measurement_reflns_used    12669
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.47
_cell_measurement_theta_min      2.21
_cell_volume                     5214(5)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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      150.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            48036
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.474
_diffrn_reflns_theta_min         1.794
_exptl_absorpt_coefficient_mu    1.497
_exptl_absorpt_correction_T_max  0.741
_exptl_absorpt_correction_T_min  0.492
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       plate
_exptl_crystal_F_000             2148
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.504
_refine_diff_density_min         -1.324
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         12669
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0511P)^2^+11.6414P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1233
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9770
_reflns_number_total             12669
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01146k2.cif
_cod_data_source_block           1_150k
_cod_depositor_comments
'Adding full bibliography for 7704487--7704490.cif.'
_cod_database_code               7704487
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.754
_shelx_estimated_absorpt_t_min   0.521
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C27-O9A
 2 with sigma of 0.02
 O9A-C27
 2.5 with sigma of 0.02
 O10A-C29
 1.25 with sigma of 0.02
 O9A-C29
 1.25 with sigma of 0.02
 O9A-O10A
 2 with sigma of 0.02
 O10A-C27
 2.5 with sigma of 0.02
3. Rigid bond restraints
 C13, C12, C14, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O10A, O9A, C29, C27, C30, C28, C26, O9, O10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O9A, C29, O10A, C27, C30, C28, C26, O9, O10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C11, C13, C12, C14, C15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
O9A \\sim C29 \\sim O10A \\sim C30 \\sim C27 \\sim C28 \\sim C26 \\sim O10
\\sim O9: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C12 \\sim C14 \\sim C13 \\sim C15 \\sim C11: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: C20(0.75) H20A(0.75) H20B(0.75) H20C(0.75) C18(0.75) H18A(0.75)
 H18B(0.75) H18C(0.75) C19(0.75) H19A(0.75) H19B(0.75) H19C(0.75) O10(0.75)
 H26A(0.25) H26B(0.25) H26C(0.25) O9(0.75) H29A(0.75) H29B(0.75) H29C(0.75)
 C19A(0.25) H19D(0.25) H19E(0.25) H19F(0.25) C20A(0.25) H20D(0.25) H20E(0.25)
 H20F(0.25) C18A(0.25) H18D(0.25) H18E(0.25) H18F(0.25) O10A(0.25) O9A(0.25)
6.a X=CH2 refined with riding coordinates:
 N11(H11A,H11B), N12(H12A,H12B), N10(H10D,H10E), N7(H7A,H7B), N9(H9D,H9E),
 N8(H8D,H8E), N3(H3D,H3E), N1(H1A,H1B), N2(H2A,H2B), N6(H6A,H6B), N5(H5D,H5E),
 N4(H4D,H4E)
6.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C15(H15A,H15B,H15C), C8(H8A,H8B,H8C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C),
 C13(H13A,H13B,H13C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C4(H4A,H4B,H4C),
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C23(H23A,H23B,H23C),
 C19A(H19D,H19E,H19F), C20A(H20D,H20E,H20F), C18A(H18D,H18E,H18F)
;
_olex2_submission_special_instructions 'No special instructions were received'