Field-Induced Slow Relaxation in a Dinuclear Dysprosium(III) Complex Based on 3-Methoxycinnamic Acid
Khalfaoui, O.; Beghidja, A.; Long, J.; Beghidja, C.; Guari, Y.; Larionova, J.; Inorganics 6 (2018) 35–; doi:10.3390/inorganics6010035

data_1556597
_publ_section_title
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 Field-Induced Slow Relaxation in a Dinuclear Dysprosium(III) Complex
 Based on 3-Methoxycinnamic Acid
;
_journal_name_full               Inorganics
_journal_page_first              35
_journal_paper_doi               10.3390/inorganics6010035
_journal_volume                  6
_journal_year                    2018
_chemical_formula_moiety         'C32 H35 Dy O11 S'
_chemical_formula_sum            'C32 H35 Dy O11 S'
_chemical_formula_weight         790.16
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                80.864(7)
_cell_angle_beta                 77.901(7)
_cell_angle_gamma                88.862(8)
_cell_formula_units_Z            2
_cell_length_a                   8.2231(11)
_cell_length_b                   12.833(2)
_cell_length_c                   17.175(2)
_cell_measurement_reflns_used    9849
_cell_measurement_temperature    273
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      3.04
_cell_volume                     1749.5(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      273
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.990
_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  0.0458
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26827
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.139
_exptl_absorpt_coefficient_mu    2.250
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       block
_exptl_crystal_F_000             794
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.266
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         7081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.003
_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^+0.3079P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0816
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5879
_reflns_number_total             7081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Inorganics-2018-6-35.cif
_cod_data_source_block           FM108B
_cod_database_code               1556597
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: S1A(0.8) H31A(0.8) H31B(0.8) H31C(0.8) H31D(0.2) H31E(0.2)
 H31F(0.2) H32D(0.2) H32A(0.8) H32E(0.2) H32B(0.8) H32F(0.2) H32C(0.8) S1B(0.2)
3.a Riding coordinates:
 C32(H32D,H32A,H32E,H32B,H32F,H32C)
3.b Rotating group:
 O11(H11A,H11B)
3.c Me refined with riding coordinates:
 C31(H31A,H31B,H31C), C31(H31D,H31E,H31F)
3.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C15(H15),
 C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C25(H25), C27(H27), C28(H28),
  C29(H29)
3.e Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C20(H20A,H20B,H20C), C30(H30A,H30B,H30C)
;