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_7120379
_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         'C34 H30 Cl2 Dy2 N2, 2(C2 H4 O0.5)'
_chemical_formula_sum            'C38 H38 Cl2 Dy2 N2 O'
_chemical_formula_weight         934.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-04-28
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-06-02 deposited with the CCDC.
2017-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.8766(7)
_cell_length_b                   7.3260(3)
_cell_length_c                   13.6863(5)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      65.327
_cell_measurement_theta_min      3.990
_cell_volume                     1892.68(13)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      100.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0882
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15829
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        61.498
_diffrn_reflns_theta_max         61.498
_diffrn_reflns_theta_min         3.989
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.399
_exptl_absorpt_correction_T_max  0.3165
_exptl_absorpt_correction_T_min  0.1477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1331 before and 0.0807 after correction. The Ratio of minimum to maximum transmission is 0.4667. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_description       plate
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.039
_exptl_crystal_size_min          0.009
_refine_diff_density_max         1.427
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.336
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         1539
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.330
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0687
_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^)+(0.0429P)^2^+21.6551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1460
_refine_ls_wR_factor_ref         0.1553
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1296
_reflns_number_total             1539
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02457f2.cif
_cod_data_source_block           cpb021
_cod_database_code               7120379
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.824
_shelx_estimated_absorpt_t_min   0.188
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C2S-C1S \\sim C2T-C1S
 with sigma of 0.02
 O1-C2S \\sim O1-C2T
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim C1S \\sim C2S \\sim C2T: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C2S) = Uanis(C2T)
4. Others
 Fixed Sof: O1(0.25) C1S(0.5) H1SA(0.25) H1SB(0.25) H1SC(0.25) H1SD(0.25)
 C2S(0.25) H2SA(0.25) H2SB(0.25) C2T(0.25) H2TA(0.25) H2TB(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C1S(H1SA,H1SB), C1S(H1SC,H1SD), C2S(H2SA,H2SB), C2T(H2TA,H2TB)
5.b Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C2(H2), C5(H5), C6(H6), C7(H7), C8(H8)
;
_shelx_res_checksum              50438
_olex2_submission_special_instructions 'No special instructions were received'