High symmetry or low symmetry, that is the question – high performance Dy(iii) single-ion magnets by electrostatic potential design
Sun, Wen-Bin; Yan, Peng-Fei; Jiang, Shang-Da; Wang, Bing-Wu; Zhang, Yi-Quan; Li, Hong-Feng; Chen, Peng; Wang, Zhe-Ming; Gao, Song; Chem. Sci. 7 (2016) 684–; doi:10.1039/C5SC02986D

data_1536870
_publ_section_title
;
 High symmetry or low symmetry, that is the question -- high performance
 Dy(iii) single-ion magnets by electrostatic potential design
;
_journal_issue                   1
_journal_name_full               'Chem. Sci.'
_journal_page_first              684
_journal_paper_doi               10.1039/C5SC02986D
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         '2(C44 H38 Br2 Dy N4 O9 Zn2), Br4 Zn'
_chemical_formula_sum            'C88 H76 Br8 Dy2 N8 O18 Zn5'
_chemical_formula_weight         2824.70
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-06-15
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_audit_update_record
;
2014-09-09 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.117(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.6367(6)
_cell_length_b                   16.8613(8)
_cell_length_c                   23.4058(12)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      27.7010
_cell_measurement_theta_min      3.4430
_cell_volume                     4836.5(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.9980
_diffrn_measured_fraction_theta_max 0.8545
_diffrn_measurement_details
;
  1 omega   -2.00   25.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7950 -115.0000 -123.0000 27

  2 omega   20.00   50.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7950  -99.0000  -60.0000 30

  3 omega  -54.00  -27.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7950  -38.0000 -120.0000 27

  4 omega    7.00   85.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7950   38.0000  -90.0000 78

  5 omega  -67.00   55.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7950  -19.0000  -90.0000 122
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0456683000
_diffrn_orient_matrix_UB_12      -0.0197683000
_diffrn_orient_matrix_UB_13      0.0059587000
_diffrn_orient_matrix_UB_21      -0.0273557000
_diffrn_orient_matrix_UB_22      0.0021169000
_diffrn_orient_matrix_UB_23      -0.0302794000
_diffrn_orient_matrix_UB_31      0.0227576000
_diffrn_orient_matrix_UB_32      -0.0370711000
_diffrn_orient_matrix_UB_33      -0.0049310000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_av_unetI/netI     0.0849
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34215
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         2.93
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.116
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2732
_refine_diff_density_max         2.254
_refine_diff_density_min         -1.295
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         10425
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0512P)^2^+11.3758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1346
_reflns_number_gt                7012
_reflns_number_total             10425
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc02986d2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1536868--1536871.cif.'
_cod_database_code               1536870
_chemical_oxdiff_formula         'C H O N Dy'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H35 of C35, H36 of C36, H41 of C41, H25 of C25, H26 of C26, H27 of C27, H28
  of C28, H30 of C30, H31 of C31, H32 of C32, H2 of C2, H22 of C22, H21 of C21,
  H20 of C20, H19 of C19, H18 of C18, H17 of C17, H12 of C12, H11 of C11, H10
  of C10, H9 of C9, H44 of C44, H5 of C5, H4 of C4
 At 1.5 times of:
  {H24A,H24B,H24C} of C24, {H3A,H3B,H3C} of C3, {H1A,H1B,H1C} of C1, {H8A,H8B,
  H8C} of C8
2. Others
 Fixed Sof: Zn3(0.5) Br4(0.5) Br5(0.5)
3.a Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C8(H8A,H8B,H8C), C24(H24A,H24B,H24C)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C44(H44), C9(H9), C10(H10), C11(H11), C12(H12),
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26),
  C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C41(H41)
;