Comparative Study of Magnetization Dynamics in Dinuclear Dysprosium Complexes Featuring Bridging Chloride or Trifluoromethanesulfonate Ligands
Burns, Corey P.; Wilkins, Branford O.; Dickie, Courtney M.; Latendresse, Trevor; Vernier, Larry; Vignesh, Kuduva R.; Bhuvanesh, Nattamai; Nippe, Michael; Chem. Commun.  (2017) –; doi:10.1039/C7CC02457F

data_7120382
_publ_section_title
;
 Comparative Study of Magnetization Dynamics in Dinuclear Dysprosium
 Complexes Featuring Bridging Chloride or Trifluoromethanesulfonate
 Ligands
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC02457F
_journal_year                    2017
_chemical_formula_moiety         '2(C18 H15 Dy F3 N O3 S), 2(C H2 Cl2)'
_chemical_formula_sum            'C38 H34 Cl4 Dy2 F6 N2 O6 S2'
_chemical_formula_weight         1259.59
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-03-14
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-03-22 deposited with the CCDC.
2017-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                92.254(4)
_cell_angle_beta                 90.145(4)
_cell_angle_gamma                107.140(4)
_cell_formula_units_Z            2
_cell_length_a                   12.2590(8)
_cell_length_b                   13.0284(9)
_cell_length_c                   13.7514(10)
_cell_measurement_reflns_used    9200
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      21.786
_cell_measurement_theta_min      2.965
_cell_volume                     2096.9(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.909
_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  0.1086
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            122841
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.482
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.966
_exptl_absorpt_correction_T_max  0.0932
_exptl_absorpt_correction_T_min  0.0530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1174 before and 0.0891 after correction.
The Ratio of minimum to maximum transmission is 0.5687.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.995
_exptl_crystal_description       block
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.138
_refine_diff_density_max         6.411
_refine_diff_density_min         -1.399
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         7353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0619
_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^)+(0.0667P)^2^+62.2040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.1690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6104
_reflns_number_total             7353
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02457f2.cif
_cod_data_source_block           cpb011
_cod_database_code               7120382
_shelx_estimated_absorpt_t_max   0.611
_shelx_estimated_absorpt_t_min   0.527
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9868(6) 0.0132(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C6B(H6BA,H6BB), C12B(H12C,H12D), C1S(H1SA,H1SB),
 C2S(H2SA,H2SB)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17), C2B(H2B), C3B(H3B), C4B(H4B), C8B(H8B), C9B(H9B),
  C10B(H10B), C11B(H11B), C14B(H14B), C15B(H15B), C16B(H16B), C17B(H17B)
;
_shelx_res_checksum              23941
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'