Equatorial coordination optimization for enhanced axiality of mononuclear Dy(iii) single-molecule magnets.
Yu, Ke-Xin; Ding, You-Song; Zhai, Yuan-Qi; Han, Tian; Zheng, Yan-Zhen; Dalton transactions (Cambridge, England : 2003) 49 (2020) 3222–3227; doi:10.1039/d0dt00011f

data_7703454
_publ_section_title
;
 Equatorial coordination optimization for enhanced axiality of mononuclear
 Dy(iii) single-molecule magnets.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3222
_journal_page_last               3227
_journal_paper_doi               10.1039/d0dt00011f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C20 H48 B2 Dy O5, C24 H20 B'
_chemical_formula_sum            'C44 H68 B3 Dy O5'
_chemical_formula_weight         871.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-02-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-29 deposited with the CCDC.	2020-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.453(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.651(3)
_cell_length_b                   13.265(3)
_cell_length_c                   24.810(6)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      27.69
_cell_measurement_theta_min      2.29
_cell_volume                     4492.5(18)
_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  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      250.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            53405
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.492
_exptl_absorpt_coefficient_mu    1.703
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1812
_refine_diff_density_max         2.558
_refine_diff_density_min         -2.987
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         7857
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      1.230
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0879
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+83.9392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2253
_refine_ls_wR_factor_ref         0.2274
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7282
_reflns_number_total             7857
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00011f2.cif
_cod_data_source_block           1_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7703452--7703454.cif.'
_cod_database_code               7703454
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 B2-H2A = B2-H2D = B2-H2C = B2-H2B = B1-H1C = B1-H1D = B1-H1B = B1-H1A
 1 with sigma of 0.02
 H1A-H1C = H1B-H1A = H1A-H1D = H1B-H1D = H1B-H1C = H1D-H1C = H2A-H2C = H2B-H2C
 = H2D-H2C = H2A-H2D = H2D-H2B = H2A-H2B
 1.8 with sigma of 0.02
 Dy1-H2B = Dy1-H2A = Dy1-H2C
 2.4 with sigma of 0.02
 Dy1-H1D = Dy1-H1B = Dy1-H1C
 2.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C10 \\sim C11 \\sim O1 \\sim C18 \\sim C19 \\sim C6 \\sim C7
\\sim C29 \\sim C30 \\sim C1: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(B1) = Uanis(B2) = Uanis(B3)
4. Rigid body (RIGU) restrains
 O4, C16, C13, C15, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C1(H1E,H1F), C2(H2E,H2F), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B)
5.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29),
 C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
  C40(H40), C41(H41), C42(H42), C43(H43), C44(H44)
;
_shelx_res_checksum              56538
_olex2_submission_special_instructions 'No special instructions were received'