Investigation of magneto-structural relation based on a series of mononuclear dysprosium single-ion magnets with high Oh symmetry
Yin, Xiuju; Li, Shixiong; Liao, Beiling; Inorganica Chimica Acta 504 (2020) 119451–; doi:10.1016/j.ica.2020.119451

data_1565248
_publ_section_title
;
 Investigation of magneto-structural relation based on a series of
 mononuclear dysprosium single-ion magnets with high Oh symmetry
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119451
_journal_paper_doi               10.1016/j.ica.2020.119451
_journal_volume                  504
_journal_year                    2020
_chemical_formula_moiety         'C22 H20 Br4 Cl3 Dy N2 O3'
_chemical_formula_sum            'C22 H20 Br4 Cl3 Dy N2 O3'
_chemical_formula_weight         948.89
_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     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 91.994(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.460(6)
_cell_length_b                   7.275(4)
_cell_length_c                   36.70(2)
_cell_measurement_reflns_used    9535
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.45
_cell_measurement_theta_min      2.22
_cell_volume                     2791(3)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0535
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            30985
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.11
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.720
_exptl_absorpt_correction_T_max  0.3028
_exptl_absorpt_correction_T_min  0.2500
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    2.258
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1788
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5678
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+3.0987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0714
_reflns_number_gt                4969
_reflns_number_total             5678
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2020-504-119452.cif
_cod_data_source_block           1018
_cod_database_code               1565248
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O3-H3
 0.85 with sigma of 0.01
 C21-H3
 1.906229 with sigma of 0.02
 Dy1-H3
 2.90564 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C21(H21a,H21b)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C3(H3a), C4(H4), C7(H7), C13(H13), C14(H14), C17(H17)
3.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C11(H11a,H11b,H11c), C22(H22a,H22b,H22c)
;