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_7245485
_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         'C78 H57 Er F15 O6 P3, C4 H8 O'
_chemical_formula_sum            'C82 H65 Er F15 O7 P3'
_chemical_formula_weight         1707.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 93.0260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3834(3)
_cell_length_b                   13.1486(3)
_cell_length_c                   45.3406(12)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.18
_cell_volume                     7372.3(3)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker Quest CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            70715
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.834
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.297
_exptl_absorpt_correction_T_max  0.3368
_exptl_absorpt_correction_T_min  0.2346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1128 before and 0.0622 after correction.
The Ratio of minimum to maximum transmission is 0.6966.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       plate
_exptl_crystal_F_000             3444
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.234
_refine_diff_density_min         -5.360
_refine_diff_density_rms         0.473
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.230
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1005
_refine_ls_number_reflns         13600
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.229
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0722
_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^)+61.1962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1482
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12267
_reflns_number_total             13600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00856d2.cif
_cod_data_source_block           4
_cod_database_code               7245485
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.659
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9926(3)
 0.0074(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
3. Restrained distances
 C24'-C17 \\sim C17'-C24
 with sigma of 0.02
 O3-C17 \\sim O3-C17'
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq, Uanis(C24') \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(F10) \\sim Ueq, 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(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(F8') \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C24) = Uanis(C24')
Uanis(C9') = Uanis(C9)
Uanis(F9) = Uanis(F9')
Uanis(F8) = Uanis(F8')
Uanis(F6) = Uanis(F6')
Uanis(F10) = Uanis(F10')
Uanis(F7) = Uanis(F7')
Uanis(C10') = Uanis(C10)
Uanis(C12') = Uanis(C12)
Uanis(C13') = Uanis(C13)
Uanis(C15) = Uanis(C15')
Uanis(C11') = Uanis(C11)
Uanis(C14) = Uanis(C14')
Uanis(C17) = Uanis(C17')
Uanis(C18') = Uanis(C18)
Uanis(C20) = Uanis(C20')
Uanis(C19) = Uanis(C19')
Uanis(C23') = Uanis(C23)
Uanis(C21') = Uanis(C21)
Uanis(C22) = Uanis(C22')
Uanis(F13') = Uanis(F13)
Uanis(F14) = Uanis(F14')
Uanis(F15) = Uanis(F15')
Uanis(F11) = Uanis(F11')
Uanis(F12') = Uanis(F12)
5. Others
 Sof(F11)=Sof(C17)=Sof(H17)=Sof(F12')=Sof(F13')=Sof(F14')=Sof(F15')=Sof(C21')=
 Sof(C22')=Sof(C23')=Sof(C18')=Sof(C19')=Sof(C20')=Sof(C24')=Sof(H24D)=
 Sof(H24E)=Sof(H24F)=1-FVAR(1)
 Sof(F12)=Sof(F13)=Sof(F14)=Sof(F15)=Sof(C18)=Sof(C19)=Sof(C20)=Sof(C21)=
 Sof(C22)=Sof(C23)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(F11')=Sof(C17')=
 Sof(H17')=FVAR(1)
 Fixed Sof: H16A(0.5) H16B(0.5) H16C(0.5) H16D(0.5) H16E(0.5) H16F(0.5)
 F6'(0.5) F7'(0.5) F8'(0.5) F9'(0.5) F10'(0.5) C9'(0.5) H9'(0.5) C10'(0.5)
 C11'(0.5) C12'(0.5) C13'(0.5) C14'(0.5) C15'(0.5) F6(0.5) F7(0.5) F8(0.5)
 F9(0.5) F10(0.5) C9(0.5) H9(0.5) C11(0.5) C12(0.5) C13(0.5) C14(0.5) C15(0.5)
 C10(0.5)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C9'(H9'), C17(H17), C9(H9), C17'(H17')
6.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB)
6.c Me refined with riding coordinates:
 C24'(H24D,H24E,H24F)
6.d Aromatic/amide H refined with riding coordinates:
 C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51),
 C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60),
  C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C68(H68), C69(H69),
 C70(H70), C71(H71), C72(H72), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78)
6.e Fitted hexagon refined as free rotating group:
 C10'(C11',C12',C13',C14',C15'), C18(C19,C20,C21,C22,C23), C11(C12,C13,C14,C15,
 C10), C21'(C22',C23',C18',C19',C20')
6.f Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C16(H16D,H16E,H16F), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              98087
_shelx_hkl_checksum              23676
_olex2_submission_special_instructions 'No special instructions were received'