Assembling two Dy2 single-molecule magnets with different energy barriers via fine-tuning the geometries of DyIII sites
Li, Dawei; Ding, Man-Man; Ge, Yu; Tello Yepes, David Felipe; Sun, Mingyuan; Najib, Muhammad Saleem; Li, Yahong; Zhang, Yi-Quan; Yao, Jin-lei; New Journal of Chemistry 44 (2020) 20634–20642; doi:10.1039/D0NJ04009F

data_7060155
_publ_section_title
;
 Assembling two Dy2 single-molecule magnets with different energy barriers
 via fine-tuning the geometries of DyIII sites
;
_journal_issue                   47
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20634
_journal_page_last               20642
_journal_paper_doi               10.1039/D0NJ04009F
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C36 H42 Dy2 N4 O16'
_chemical_formula_sum            'C36 H42 Dy2 N4 O16'
_chemical_formula_weight         1111.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-12 deposited with the CCDC.	2020-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0333(14)
_cell_length_b                   9.0499(7)
_cell_length_c                   23.067(2)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.547
_cell_measurement_theta_min      3.055
_cell_volume                     3973.3(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            13445
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.598
_diffrn_reflns_theta_min         2.492
_exptl_absorpt_coefficient_mu    3.809
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1177 before and 0.0484 after correction. The Ratio of minimum to maximum transmission is 0.6247. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_description       block
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.173
_refine_diff_density_min         -3.982
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.212
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4539
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.212
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0436P)^2^+44.8969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1522
_refine_ls_wR_factor_ref         0.1574
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3898
_reflns_number_total             4539
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04009f2.cif
_cod_data_source_block           t
_cod_original_cell_volume        3973.2(5)
_cod_database_code               7060155
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,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
 C18-H3
 1.908489 with sigma of 0.02
 Dy1-H3
 2.854668 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C4(H4), C10(H10), C16(H16), C15(H15), C5(H5), C6(H6)
3.c Idealised Me refined as rotating group:
 C18(H18A,H18C,H18B), C14(H14A,H14B,H14C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              46359
_olex2_submission_special_instructions 'No special instructions were received'