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_7704488
_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                 91.047(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.739(7)
_cell_length_b                   13.289(5)
_cell_length_c                   22.613(8)
_cell_measurement_reflns_used    7288
_cell_measurement_temperature    400
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.21
_cell_volume                     5330(3)
_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      400.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0688
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38469
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.568
_diffrn_reflns_theta_min         1.777
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.465
_exptl_absorpt_correction_T_max  0.644
_exptl_absorpt_correction_T_min  0.596
_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    1.282
_exptl_crystal_description       block
_exptl_crystal_F_000             2148
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.013
_refine_diff_density_min         -0.925
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         12132
_refine_ls_number_restraints     237
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0635P)^2^+1.2971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1348
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7288
_reflns_number_total             12132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01146k2.cif
_cod_data_source_block           1_400k
_cod_depositor_comments
'Adding full bibliography for 7704487--7704490.cif.'
_cod_database_code               7704488
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.668
_shelx_estimated_absorpt_t_min   0.528
_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
 C40-C9
 1.55 with sigma of 0.02
 O11A-C26
 1.3 with sigma of 0.02
 O10A-C26
 1.25 with sigma of 0.02
 O10A-C14
 2.5 with sigma of 0.02
 O11A-C14
 2.6 with sigma of 0.02
 C28-O11A
 4.5 with sigma of 0.02
 O10A-O11A
 2.1 with sigma of 0.02
3. Rigid bond restraints
 C26, C14, C22, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C15, C34, C33, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O10A, C26, O11A, C27, C14, C22, C10, O10, O11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C29 \\sim C33 \\sim C34 \\sim C15: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C39 \\sim C40 \\sim C38 \\sim C9: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C34 \\sim C15 \\sim C33 \\sim C29: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C26 \\sim C14 \\sim C27 \\sim C22 \\sim C10 \\sim O10 \\sim O11: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C11 \\sim C28 \\sim C36 \\sim C30 \\sim C32 \\sim C37 \\sim C35 \\sim C6:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C29 \\sim C15 \\sim C34 \\sim C41 \\sim C42 \\sim C33: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
O10A \\sim O11A \\sim C26 \\sim C14 \\sim C27 \\sim C22 \\sim C10 \\sim O10
\\sim O11: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C40) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: O10(0.875) O11(0.875) H10A(0.125) H10B(0.125) H10C(0.125) C17(0.6)
 H17A(0.6) H17B(0.6) H17C(0.6) C20(0.6) H20A(0.6) H20B(0.6) H20C(0.6) C25(0.6)
 H25A(0.6) H25B(0.6) H25C(0.6) H26A(0.875) H26B(0.875) H26C(0.875) C28(0.66667)
 H28A(0.66667) H28B(0.66667) H28C(0.66667) C30(0.66667) H30A(0.66667)
 H30B(0.66667) H30C(0.66667) C32(0.66667) H32A(0.66667) H32B(0.66667)
 H32C(0.66667) C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C34(0.5) H34A(0.5)
 H34B(0.5) H34C(0.5) C35(0.33333) H35A(0.33333) H35B(0.33333) H35C(0.33333)
 C36(0.33333) H36A(0.33333) H36B(0.33333) H36C(0.33333) C37(0.33333)
 H37A(0.33333) H37B(0.33333) H37C(0.33333) C38(0.4) H38A(0.4) H38B(0.4)
 H38C(0.4) C39(0.4) H39A(0.4) H39B(0.4) H39C(0.4) C40(0.4) H40A(0.4) H40B(0.4)
 H40C(0.4) C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5) C42(0.5) H42A(0.5) H42B(0.5)
 H42C(0.5) O11A(0.125) O10A(0.125)
6.a X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B), N5(H5A,H5B), N6(H6A,H6B),
 N7(H7A,H7B), N8(H8A,H8B), N9(H9A,H9B), N10(H10D,H10E), N11(H11A,H11B),
 N12(H12A,H12B)
6.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C),
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,
 H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C)
;
_olex2_submission_special_instructions 'No special instructions were received'