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_7703453
_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
'C12 H32 B2 Dy O6, C20 H40 Na O8, 2(C24 H20 B)'
_chemical_formula_sum            'C80 H112 B4 Dy Na O14'
_chemical_formula_weight         1526.42
_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             2019-02-08
_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                 101.305(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.208(4)
_cell_length_b                   18.045(6)
_cell_length_c                   20.555(7)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.23
_cell_volume                     4077(2)
_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
;
%$getVar(solution_reference_short)%
;
_diffrn_ambient_temperature      250.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20977
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         1.515
_exptl_absorpt_coefficient_mu    0.981
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1602
_exptl_crystal_size_max          0.687
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.136
_refine_diff_density_max         1.198
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         7925
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0549P)^2^+4.0465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1084
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6106
_reflns_number_total             7925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00011f2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7703452--7703454.cif.'
_cod_database_code               7703453
_shelx_shelxl_version_number     2018/3
_publ_section_exptl
;
Any special experimental details
;
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.552
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C40-O7 = C37-O7
 1.43 with sigma of 0.01
 C37-C38 = C38-C39 = C39-C40
 1.5 with sigma of 0.01
 C37-C39 = C38-C40
 2.4 with sigma of 0.01
 B2-H2A = B2-H2D = B2-H2C = B2-H2B
 1 with sigma of 0.02
 H2A-H2B = H2C-H2A = H2C-H2B = H2D-H2B = H2D-H2A = H2D-H2C
 1.8 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40)
\\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(C37) = Uanis(C38) = Uanis(C39) = Uanis(C40) = Uanis(O7)
4.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C39(H39A,H39B),
  C40(H40A,H40B), C38(H38A,H38B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24)
;
_shelx_res_checksum              27066
_olex2_submission_special_instructions 'No special instructions were received'