Effect on the geometry over the slow relaxation of the magnetization in a series of Erbium(III) complexes based on halogenated ligands.
Long, Jérôme; Lyubov, Dmitry; Kissel, Alexander; Gogolev, Ilia A.; Tyutyunov, Andrey A.; Nelyubina, Yulia V.; Salles, Fabrice; Guari, Yannick; Cherkasov, Anton; Larionova, Joulia; Trifonov, Alexander; CrystEngComm  (2022) –; doi:10.1039/D2CE00856D

data_7245482
_publ_section_title
;
 Effect on the geometry over the slow relaxation of the magnetization in a
 series of Erbium(III) complexes based on halogenated ligands.
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00856D
_journal_year                    2022
_chemical_formula_moiety         'C63 H45 Er1 F18 O5.023 P2'
_chemical_formula_sum            'C63 H45 Er F18 O5.02 P2'
_chemical_formula_weight         1453.56
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-05-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-05-27 deposited with the CCDC.	2022-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   18.885(12)
_cell_length_b                   18.885(12)
_cell_length_c                   28.24(2)
_cell_measurement_reflns_used    2215
_cell_measurement_temperature    120
_cell_measurement_theta_max      23.99
_cell_measurement_theta_min      2.16
_cell_volume                     8722(10)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Quest D8'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.4521
_diffrn_reflns_av_unetI/netI     0.1878
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            41894
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         1.439
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.607
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_correction_T_min  0.2435
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1630 before and 0.1075 after correction.
The Ratio of minimum to maximum transmission is 0.5624.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       needle
_exptl_crystal_F_000             4339
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.672
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.208
_refine_ls_extinction_coef       0.0196(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3415
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.2037
_refine_ls_R_factor_gt           0.1080
_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^)+(0.1339P)^2^+76.4698P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2474
_refine_ls_wR_factor_ref         0.3017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1610
_reflns_number_total             3415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00856d2.cif
_cod_data_source_block           2
_cod_original_cell_volume        8722(13)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7245482
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.856
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 P2-O3 \\sim P2-O4
 with sigma of 0.02
 P1-C10' \\sim P1-C10
 with sigma of 0.02
 C2-C1 \\sim C2'-C1
 with sigma of 0.02
 P2-C16' \\sim P2-C16
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C19) \\sim Ueq, Uanis(C19') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C18) \\sim Ueq, Uanis(C16') \\sim Ueq, Uanis(C17') \\sim Ueq, Uanis(C20')
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C19) \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15') \\sim Ueq, Uanis(C11') \\sim Ueq,
Uanis(C12') \\sim Ueq, Uanis(C13') \\sim Ueq, Uanis(C14') \\sim Ueq,
Uanis(C10') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C2') \\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
Uanis(C10) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O3) = Uanis(O4)
Uanis(C2') = Uanis(C2)
Uanis(C6) = Uanis(C6')
Uanis(C5) = Uanis(C5')
Uanis(C3') = Uanis(C3)
Uanis(C7) = Uanis(C7')
Uanis(C4') = Uanis(C4)
Uanis(C19) = Uanis(C19')
Uanis(C18') = Uanis(C18)
Uanis(C20) = Uanis(C20')
Uanis(C21') = Uanis(C21)
Uanis(C16') = Uanis(C16)
Uanis(C17') = Uanis(C17)
Uanis(C14') = Uanis(C14)
Uanis(C12') = Uanis(C12)
Uanis(C13') = Uanis(C13)
Uanis(C11') = Uanis(C11)
Uanis(C15') = Uanis(C15)
Uanis(C10) = Uanis(C10')
4. Others
 Sof(C2)=Sof(C3')=Sof(H3')=Sof(C4')=Sof(H4')=Sof(C5')=Sof(H5')=Sof(C6')=
 Sof(H6')=Sof(C7')=Sof(H7')=1-FVAR(1)
 Sof(C2')=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=
 Sof(C7)=Sof(H7)=FVAR(1)
 Sof(C15')=Sof(H15')=Sof(C10')=Sof(C11')=Sof(H11')=Sof(C12')=Sof(H12')=
 Sof(C13')=Sof(H13')=Sof(C14')=Sof(H14')=1-FVAR(2)
 Sof(C10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=Sof(C14)=
 Sof(H14)=Sof(C15)=Sof(H15)=FVAR(2)
 Sof(C16)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=
 Sof(H20)=Sof(C21)=Sof(H21)=1-FVAR(3)
 Sof(C21')=Sof(H21')=Sof(C16')=Sof(C17')=Sof(H17')=Sof(C18')=Sof(H18')=
 Sof(C19')=Sof(H19')=Sof(C20')=Sof(H20')=FVAR(3)
 Fixed Sof: O3(0.11111) O4(0.23)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C21'(H21'), C17'(H17'), C18'(H18'), C19'(H19'), C20'(H20'),
  C3'(H3'), C4'(H4'), C5'(H5'), C6'(H6'), C7'(H7'), C15'(H15'), C11'(H11'),
 C12'(H12'), C13'(H13'), C14'(H14'), C17(H17), C18(H18), C19(H19), C20(H20),
 C21(H21)
5.b Fitted hexagon refined as free rotating group:
 C2'(C3,C4,C5,C6,C7), C10(C11,C12,C13,C14,C15), C21'(C16',C17',C18',C19',C20'),
  C2(C3',C4',C5',C6',C7'), C15'(C10',C11',C12',C13',C14'), C16(C17,C18,C19,C20,
 C21)
;
_shelx_res_checksum              14652
_shelx_hkl_checksum              13160
_olex2_submission_special_instructions 'No special instructions were received'