Hard versus soft: zero-field dinuclear Dy(iii) oxygen bridged SMM and theoretical predictions of the sulfur and selenium analogues.
Vignesh, Kuduva R.; Alexandropoulos, Dimitris I.; Dolinar, Brian S.; Dunbar, Kim R.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2872–2876; doi:10.1039/c9dt00324j

data_7048759
_publ_section_title
;
 Hard versus soft: zero-field dinuclear Dy(iii) oxygen bridged SMM and
 theoretical predictions of the sulfur and selenium analogues.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2872
_journal_page_last               2876
_journal_paper_doi               10.1039/c9dt00324j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C46 H58 Dy2 N2 O14, 2(N O3), 4(C2 H3 N)'
_chemical_formula_sum            'C54 H70 Dy2 N8 O20'
_chemical_formula_weight         1476.18
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-11-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-21 deposited with the CCDC.
2019-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                63.5140(10)
_cell_angle_beta                 85.6460(10)
_cell_angle_gamma                80.8900(10)
_cell_formula_units_Z            1
_cell_length_a                   10.5842(3)
_cell_length_b                   12.0661(4)
_cell_length_c                   12.7702(4)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      25.71
_cell_measurement_theta_min      2.56
_cell_volume                     1441.27(8)
_computing_cell_refinement       'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_data_collection       'APEX3(Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON area detector'
_diffrn_measurement_method       '0.5\ \w and 0.5\ \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24328
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.719
_diffrn_reflns_theta_min         2.528
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.655
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0858 before and 0.0364 after correction.
The Ratio of minimum to maximum transmission is 0.8564.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             742
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         5474
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0172
_refine_ls_R_factor_gt           0.0158
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0189P)^2^+0.9572P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0381
_refine_ls_wR_factor_ref         0.0385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5271
_reflns_number_total             5474
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00324j2.cif
_cod_data_source_block           vig42_mecn_0m_a
_cod_depositor_comments
'Adding full bibliography for 7048759--7048760.cif.'
_cod_database_code               7048759
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.619
_shelx_estimated_absorpt_t_min   0.416
_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
 O4-H4
 0.87 with sigma of 0.01
 O2-H2
 0.87 with sigma of 0.01
 O3-H3
 0.87 with sigma of 0.01
 C8-H4
 1.919943 with sigma of 0.02
 Dy1-H4
 3.055482 with sigma of 0.02
 C4-H2
 1.916833 with sigma of 0.02
 Dy1-H2
 3.102054 with sigma of 0.02
 C6-H3
 1.920327 with sigma of 0.02
 Dy1-H3
 3.079967 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C16(H16), C19(H19), C20(H20),
 C21(H21), C22(H22), C23(H23)
3.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C)
3.d Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_shelx_res_checksum              54060
_olex2_submission_special_instructions 'No special instructions were received'