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_7245483
_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         'C50 H46 Cl3 Er F6 O5'
_chemical_formula_sum            'C50 H46 Cl3 Er F6 O5'
_chemical_formula_weight         1114.48
_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                 92.7490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7102(3)
_cell_length_b                   15.8031(3)
_cell_length_c                   18.5149(3)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.10
_cell_measurement_theta_min      2.17
_cell_volume                     4591.40(14)
_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      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_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  0.0430
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            52446
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.829
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.074
_exptl_absorpt_correction_T_max  0.1561
_exptl_absorpt_correction_T_min  0.0895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1192 before and 0.0529 after correction.
The Ratio of minimum to maximum transmission is 0.5734.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       plate
_exptl_crystal_F_000             2236
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.160
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         10022
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0256
_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^)+(0.0216P)^2^+5.0114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8557
_reflns_number_total             10022
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00856d2.cif
_cod_data_source_block           1
_cod_database_code               7245483
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.530
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 Cl3'-C42 \\sim Cl3-C42
 with sigma of 0.02
 F5-C42 \\sim F6'-C42
 with sigma of 0.02
 F5'-C42 \\sim F6-C42
 with sigma of 0.02
 C6S-C7S \\sim C7S'-C6S'
 with sigma of 0.02
 C7S-C8S \\sim C7S'-C8S
 with sigma of 0.02
 C6S-C5S \\sim C6S'-C5S
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl3') = Uanis(Cl3)
Uanis(F6') = Uanis(F5)
Uanis(F5') = Uanis(F6)
Uanis(C6S') = Uanis(C6S)
Uanis(C7S) = Uanis(C7S')
4. Others
 Sof(Cl3)=Sof(F5)=Sof(F6)=1-FVAR(1)
 Sof(Cl3')=Sof(F5')=Sof(F6')=FVAR(1)
 Sof(H5SC)=Sof(H5SD)=Sof(H8SC)=Sof(H8SD)=Sof(C6S')=Sof(H6SC)=Sof(H6SD)=
 Sof(C7S')=Sof(H7SC)=Sof(H7SD)=1-FVAR(2)
 Sof(H5SA)=Sof(H5SB)=Sof(H8SA)=Sof(H8SB)=Sof(C6S)=Sof(H6SB)=Sof(H6SA)=Sof(C7S)=
 Sof(H7SA)=Sof(H7SB)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,
 H5SB), C5S(H5SC,H5SD), C8S(H8SA,H8SB), C8S(H8SC,H8SD), C6S(H6SB,H6SA),
 C7S(H7SA,H7SB), C6S'(H6SC,H6SD), C7S'(H7SC,H7SD)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24),
  C25(H25), C26(H26), C27(H27), C31(H31), C32(H32), C33(H33), C34(H34),
 C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41)
;
_shelx_res_checksum              97385
_shelx_hkl_checksum              18795
_olex2_submission_special_instructions 'No special instructions were received'