Magnetic behavior of the novel pentagonal-bipyramidal erbium(iii) complex (Et3NH)[Er(H2DAPS)Cl2]: high-frequency EPR study and crystal-field analysis
Spillecke, Lena; Koo, Changhyun; Maximova, Olga; Mironov, Vladimir S.; Kopotkov, Vycheslav A.; Korchagin, Denis V.; Vasiliev, Alexander N.; Yagubskii, Eduard B.; Klingeler, Rüdiger; Dalton Transactions  (2021) –; doi:10.1039/D1DT03228C

data_7709000
_publ_section_title
;
 Magnetic behavior of the novel pentagonal-bipyramidal erbium(iii) complex
 (Et3NH)[Er(H2DAPS)Cl2]: high-frequency EPR study and crystal-field
 analysis
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03228C
_journal_year                    2021
_chemical_formula_moiety         'C23 H19 Cl2 Er N5 O4, C6 H16 N'
_chemical_formula_sum            'C29 H35 Cl2 Er N6 O4'
_chemical_formula_weight         769.79
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-10-31 deposited with the CCDC.	2021-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7290(5)
_cell_length_b                   14.8702(4)
_cell_length_c                   11.1918(4)
_cell_measurement_reflns_used    2947
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      31.4645
_cell_measurement_theta_min      2.8304
_cell_volume                     3116.96(16)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5094
_diffrn_reflns_point_group_measured_fraction_full 0.822
_diffrn_reflns_point_group_measured_fraction_max 0.795
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.065
_diffrn_reflns_theta_min         3.290
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.908
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_description       'rectangular blocks'
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.649
_refine_diff_density_min         -1.075
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details
;
 Flack x determined using 956 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.035(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3427
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0132P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0533
_refine_ls_wR_factor_ref         0.0551
_reflns_Friedel_coverage         0.518
_reflns_Friedel_fraction_full    0.626
_reflns_Friedel_fraction_max     0.571
_reflns_number_gt                3085
_reflns_number_total             3427
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03228c2.cif
_cod_data_source_block           Er
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'direct methods' was
changed to 'direct'.

data item '_atom_sites_solution_secondary' value 'diff Fourier map'
was changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        3116.95(16)
_cod_database_code               7709000
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              99151
_shelx_hkl_checksum              90845