Six-coordinated dinuclear lanthanide(III) amide complexes: investigation of magnetization relaxation dynamics and their electronic structures.
Rasamsetty, Amaleswari; Mehta, Sakshi; Ansari, Kamal Uddin; Kumar, Pardeep; Mondal, Abhishake; Shanmugam, Maheswaran; Dalton transactions (Cambridge, England : 2003) 51 (2021) 63–68; doi:10.1039/d1dt03708k

data_7708909
_publ_section_title
;
 Six-coordinated dinuclear lanthanide(III) amide complexes: investigation
 of magnetization relaxation dynamics and their electronic structures.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              63
_journal_page_last               68
_journal_paper_doi               10.1039/d1dt03708k
_journal_volume                  51
_journal_year                    2021
_chemical_formula_moiety         'C54 H100 Cl6 Dy2 Li2 N2 O6 Si2'
_chemical_formula_sum            'C54 H100 Cl6 Dy2 Li2 N2 O6 Si2'
_chemical_formula_weight         1481.11
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-04-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-06-03 deposited with the CCDC.	2021-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8807(2)
_cell_length_b                   17.2088(2)
_cell_length_c                   20.8678(3)
_cell_measurement_reflns_used    46728
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.2870
_cell_measurement_theta_min      1.9790
_cell_volume                     6780.24(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -101.50  22.00   0.50    2.00    --  -20.00   0.00 108.00  247
  2  \w    -73.00 -43.00   0.50    2.00    --  -20.00 -72.00-108.00   60
  3  \w    -20.00  10.00   0.50    2.00    --  -20.00  72.00  36.00   60
  4  \w    -67.50  16.00   0.50    2.00    --  -20.00   0.00-108.00  167
  5  \w   -109.00 -79.00   0.50    2.00    --  -20.00   0.00-180.00   60
  6  \w    -59.00 -25.50   0.50    2.00    --  -20.00  72.00 108.00   67
  7  \w    -11.00  42.00   0.50    2.00    --  -20.00  72.00-180.00  106
  8  \w    -56.50  70.00   0.50    2.00    --  -20.00   0.00 -36.00  253
  9  \w    -72.00 -40.00   0.50    2.00    --  -20.00 -72.00  36.00   64
 10  \w    -34.50  53.50   0.50    2.00    --  -20.00  72.00-108.00  176
 11  \w   -110.00 -76.50   0.50    2.00    --  -20.00   0.00  36.00   67
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0214968000
_diffrn_orient_matrix_UB_12      -0.0231133000
_diffrn_orient_matrix_UB_13      0.0203309000
_diffrn_orient_matrix_UB_21      0.0157335000
_diffrn_orient_matrix_UB_22      -0.0175930000
_diffrn_orient_matrix_UB_23      -0.0272467000
_diffrn_orient_matrix_UB_31      0.0264832000
_diffrn_orient_matrix_UB_32      0.0292364000
_diffrn_orient_matrix_UB_33      -0.0003438000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            81881
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.230
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.502
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       block
_exptl_crystal_F_000             3016
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.296
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         5976
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.289
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0096P)^2^+42.2400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0930
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5476
_reflns_number_total             5976
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03708k2.cif
_cod_data_source_block           Complex2_Dy
_cod_depositor_comments
'Adding full bibliography for 7708907--7708909.cif.'
_cod_original_cell_volume        6780.25(15)
_cod_database_code               7708909
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.705
_shelx_estimated_absorpt_t_min   0.635
_reflns_odcompleteness_completeness 94.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.12
_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
2. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq, Uanis(C0) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C1AA)
\\sim Ueq, Uanis(C9B) \\sim Ueq, Uanis(O3A) \\sim Ueq, Uanis(C9A) \\sim Ueq,
Uanis(C2AA) \\sim Ueq, Uanis(C3AA) \\sim Ueq, Uanis(C4AA) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.001
3. Others
 Sof(O3)=Sof(C0)=Sof(H0A)=Sof(H0B)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(C1AA)=
 Sof(H1AA)=Sof(H1AB)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=1-FVAR(1)
 Sof(O3A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=Sof(C3AA)=
 Sof(H3AA)=Sof(H3AB)=Sof(C4AA)=Sof(H4AA)=Sof(H4AB)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10)
4.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C16(H16A,H16B), C13(H13A,H13B), C15(H15A,H15B), C20(H20A,
 H20B), C17(H17A,H17B), C19(H19A,H19B), C0(H0A,H0B), C18(H18A,H18B), C0AA(H0AA,
 H0AB), C1AA(H1AA,H1AB), C9B(H9BA,H9BB), C9A(H9AA,H9AB), C2AA(H2AA,H2AB),
 C3AA(H3AA,H3AB), C4AA(H4AA,H4AB)
4.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C3(H3)
4.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C8(H8A,H8B,H8C), C21(H21A,H21B,
 H21C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              41021
_shelx_hkl_checksum              39163
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.255
_oxdiff_exptl_absorpt_empirical_full_min 0.689