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_1536869
_publ_section_title
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 High symmetry or low symmetry, that is the question -- high performance
 Dy(iii) single-ion magnets by electrostatic potential design
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_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
'0.5(C45 H40 Br2 Dy N4 O9 Zn2), 0.5(Br), 1.5(O)'
_chemical_formula_sum            'C45 H40 Br3 Cl0 Dy N4 O12 Zn2'
_chemical_formula_weight         1361.78
_chemical_name_systematic
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 ? 
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_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-09-09
_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                92.178(3)
_cell_angle_beta                 108.240(3)
_cell_angle_gamma                99.096(3)
_cell_formula_units_Z            2
_cell_length_a                   10.6898(4)
_cell_length_b                   15.3759(6)
_cell_length_c                   16.5328(4)
_cell_measurement_temperature    293(2)
_cell_volume                     2537.31(16)
_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.
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_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_unetI/netI     0.0932
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22070
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.82
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.819
_exptl_absorpt_correction_T_max  0.5127
_exptl_absorpt_correction_T_min  0.4458
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1330
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         4.211
_refine_diff_density_min         -2.064
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         9982
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0684
_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^)+(0.0987P)^2^+11.3371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1779
_refine_ls_wR_factor_ref         0.1924
_reflns_number_gt                7823
_reflns_number_total             9982
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc02986d2.cif
_cod_data_source_block           v
_cod_depositor_comments
'Adding full bibliography for 1536868--1536871.cif.'
_cod_original_cell_volume        2537.31(15)
_cod_database_code               1536869
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  H27 of C27, H30A of C30, H35 of C35, H37 of C37, H38 of C38, H39 of C39,
  H42 of C42, H43 of C43, H45 of C45, H44 of C44, H7A of C7, H32A of C32, H9A
  of C9, H10 of C10, H11 of C11, H14 of C14, H18 of C18, H19 of C19, H20 of C20,
   H21 of C21, H53 of C22, H23 of C23, H25 of C25, H26 of C26
 At 1.5 times of:
  {H31A,H31B,H31C} of C31, {H34A,H34B,H34C} of C34, {H3A,H3B,H3C} of C3, {H2A,
  H2B,H2C} of C2, {H1A,H1B,H1C} of C1, H9 of O9
2. Restrained distances
 O9-H9
 0.85 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints

4. Others
 Fixed Sof: Br4(0.5) Br3(0.5)
5.a Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C31(H31A,H31B,H31C)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7A), C9(H9A), C10(H10), C11(H11), C14(H14), C18(H18), C19(H19), C20(H20),
 C21(H21), C22(H53), C23(H23), C25(H25), C26(H26), C27(H27), C30(H30A),
 C32(H32A), C35(H35), C37(H37), C38(H38), C39(H39), C42(H42), C43(H43),
 C45(H45), C44(H44)
5.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C)
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