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_7703452
_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 H36 B3 Dy O3'
_chemical_formula_sum            'C12 H36 B3 Dy O3'
_chemical_formula_weight         423.34
_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             2019-02-12
_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
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2218(3)
_cell_length_b                   14.4491(4)
_cell_length_c                   14.5213(4)
_cell_measurement_reflns_used    5840
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.62
_cell_volume                     1934.92(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11515
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.645
_diffrn_reflns_theta_min         2.620
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.861
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             852
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         2248
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.182
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0253
_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^)+(0.0398P)^2^+2.3534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0833
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1609
_reflns_number_total             2248
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00011f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7703452--7703454.cif.'
_cod_database_code               7703452
_shelx_shelxl_version_number     2018/3
_publ_section_exptl
;
Any special experimental details
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 C5-C6
 1.45 with sigma of 0.01
 C5-O2
 1.4 with sigma of 0.01
 H2b-H2a_$1 = H2a_$1-H2a = H2b-H2a = H2b_$1-H2a = H2b_$1-H2a_$1 = H2b_$1-H2b
 1.8 with sigma of 0.02
 B2-H2b_$1 = B2-H2a = B2-H2b = B2-H2a_$1
 1 with sigma of 0.02
 B1-H1d = B1-H1c = B1-H1b = B1-H1a
 1 with sigma of 0.02
 H1c-H1b = H1c-H1a = H1b-H1a = H1d-H1b = H1d-H1a = H1d-H1c
 1.8 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C1(H1e,H1f), C2(H2c,H2d), C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b), C6(H6a,H6b)
;
_shelx_res_checksum              72307
_olex2_submission_special_instructions 'No special instructions were received'