Identical anomalous Raman relaxation exponent in a family of single ion magnets: towards reliable Raman relaxation determination?
Handzlik, Gabriela; Magott, Michał; Arczyński, Mirosław; Sheveleva, Alena M.; Tuna, Floriana; Baran, Stanisław; Pinkowicz, Dawid; Dalton transactions (Cambridge, England : 2003) 49 (2020) 11942–11949; doi:10.1039/d0dt02439b

data_7705132
_publ_section_title
;
 Identical anomalous Raman relaxation exponent in a family of single ion
 magnets: towards reliable Raman relaxation determination?
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11942
_journal_page_last               11949
_journal_paper_doi               10.1039/d0dt02439b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C48 H32 Er N8 O8, 3(N O3)'
_chemical_formula_sum            'C48 H32 Er N11 O17'
_chemical_formula_weight         1202.10
_chemical_properties_physical
'easy loss of crystallization solvent (methanol)'
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-08-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-08 deposited with the CCDC.	2020-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3972(16)
_cell_length_b                   15.3972(16)
_cell_length_c                   22.418(4)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    161(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.61
_cell_volume                     5314.7(12)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8QuestEco Photon50'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            22766
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.359
_diffrn_reflns_theta_min         2.608
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.659
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5277
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1008 before and 0.0814 after correction.
The Ratio of minimum to maximum transmission is 0.7079.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       block
_exptl_crystal_F_000             2404
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.23
_refine_diff_density_max         2.616
_refine_diff_density_min         -1.664
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         2793
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0918P)^2^+31.9789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1421
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2464
_reflns_number_total             2793
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02439b2.cif
_cod_data_source_block           gh283_0m_a_sq
_cod_depositor_comments
'Adding full bibliography for 7705131--7705134.cif.'
_cod_original_cell_volume        5314.8(14)
_cod_database_code               7705132
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.702
_shelx_estimated_absorpt_t_min   0.557
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O4A-N4
 1.25 with sigma of 0.005
 O4B-N4
 1.25 with sigma of 0.005
 N3-O3B
 1.25 with sigma of 0.005
 N3-O3A
 1.25 with sigma of 0.005
 N5-O5A
 1.25 with sigma of 0.005
 O5B-N5
 1.25 with sigma of 0.005
 N3-O3C
 1.25 with sigma of 0.005
 O4B-O4A
 2.16 with sigma of 0.005
 O3A-O3B
 2.16 with sigma of 0.005
 O5B-O5A
 2.16 with sigma of 0.005
 O3A-O3C
 2.16 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(N3) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(N4) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O4B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(N5) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O5B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O3A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
: with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Others
 Fixed Sof: O5A(0.125) O4A(0.125) O3B(0.5) O5B(0.25) O4B(0.25)
 Fixed Uiso: O3C(0.2)
5.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C6(H6), C5(H5), C3(H3), C2(H2)
;
_shelx_res_checksum              59062
_shelx_fab_checksum              79054
_olex2_submission_special_instructions 'No special instructions were received'