Slow magnetic relaxation in a {EuCu<sub>5</sub>} metallacrown.
Wang, Jin; Ruan, Ze-Yu; Li, Quan-Wen; Chen, Yan-Cong; Huang, Guo-Zhang; Liu, Jun-Liang; Reta, Daniel; Chilton, Nicholas F.; Wang, Zhen-Xing; Tong, Ming-Liang; Dalton transactions (Cambridge, England : 2003) 48 (2019) 1686–1692; doi:10.1039/c8dt04814b

data_7048584
_publ_section_title
;
 Slow magnetic relaxation in a {EuCu<sub>5</sub>} metallacrown.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1686
_journal_page_last               1692
_journal_paper_doi               10.1039/c8dt04814b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'C89 H65 Cu5 Lu N15 O14, C5 H5 N, H2 O, C F3 O3 S'
_chemical_formula_sum            'C95 H76 Cu5 F3 Lu N16 O20 S'
_chemical_formula_weight         2343.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-21 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                108.072(2)
_cell_angle_beta                 106.380(2)
_cell_angle_gamma                93.023(2)
_cell_formula_units_Z            2
_cell_length_a                   13.3798(6)
_cell_length_b                   18.4376(8)
_cell_length_c                   21.1189(10)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.23
_cell_volume                     4695.3(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX3 v2016.1-0'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'Bruker PHOTON 100 CMOS detector'
_diffrn_detector_type            'CMOS active pixel sensor detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            100153
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.548
_diffrn_reflns_theta_min         1.068
_diffrn_source                   'I\mS microfocus'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.261
_exptl_absorpt_correction_T_max  0.0949
_exptl_absorpt_correction_T_min  0.0561
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2354
_exptl_crystal_size_max          0.117
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.022
_refine_diff_density_max         3.502
_refine_diff_density_min         -1.469
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1246
_refine_ls_number_reflns         21581
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0499P)^2^+14.7889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1167
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17728
_reflns_number_total             21581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04814b2.cif
_cod_data_source_block           LuCu5
_cod_depositor_comments
'Adding full bibliography for 7048583--7048584.cif.'
_cod_database_code               7048584
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.778
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
2. Restrained distances
 C95-F2 = C95-F3
 1.35 with sigma of 0.01
3. Restrained planarity
 N12, C70, C71, C72, C73, C74
 with sigma of 0.01
4. Rigid bond restraints
 N12, C70, C71, C72, C73, C74
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N12, C70, C71
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 S1, O17, S1, C95, F2, C95
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Uiso/Uaniso restraints and constraints
Uanis(C72) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C93)
\\sim Ueq, Uanis(O16) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C70) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C95) \\sim Ueq: with sigma of
0.002 and sigma for terminal atoms of 0.004
Uanis(S1) = Uanis(C95)
6.a Riding coordinates:
 O1W(H1WA,H1WB)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14),
 C15(H15), C17(H17), C18(H18), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27),
  C28(H28), C32(H32), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38),
 C42(H42), C43(H43), C44(H44), C45(H45), C47(H47), C48(H48), C52(H52), C53(H53),
  C54(H54), C55(H55), C57(H57), C59(H59), C60(H60), C61(H61), C62(H62),
 C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70), C71(H71),
  C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78),
 C79(H79), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84), C85(H85), C86(H86),
  C87(H87), C88(H88), C89(H89), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94)
;
_shelx_res_checksum              13005
_shelx_fab_checksum              23120
_olex2_submission_special_instructions 'No special instructions were received'