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_7708908
_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 Li2 N2 O6 Si2 Y2'
_chemical_formula_sum            'C54 H100 Cl6 Li2 N2 O6 Si2 Y2'
_chemical_formula_weight         1333.93
_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     dual
_audit_creation_date             2021-03-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_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                   18.8863(14)
_cell_length_b                   17.2224(17)
_cell_length_c                   20.8711(19)
_cell_measurement_reflns_used    4134
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.7960
_cell_measurement_theta_min      1.9910
_cell_volume                     6788.7(10)
_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 (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      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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   -110.00  19.00   0.50    8.00    --  -20.00 -72.00 108.00  258
  2  \w    -18.50  19.00   0.50    8.00    --  -20.00 -72.00 -36.00   75
  3  \w   -102.00 -76.00   0.50    8.00    --  -20.00   0.00 108.00   52
;
_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      -0.0125569000
_diffrn_orient_matrix_UB_12      -0.0167261000
_diffrn_orient_matrix_UB_13      -0.0289128000
_diffrn_orient_matrix_UB_21      0.0013185000
_diffrn_orient_matrix_UB_22      -0.0373633000
_diffrn_orient_matrix_UB_23      0.0142514000
_diffrn_orient_matrix_UB_31      -0.0353679000
_diffrn_orient_matrix_UB_32      0.0045506000
_diffrn_orient_matrix_UB_33      0.0107619000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1724
_diffrn_reflns_av_unetI/netI     0.1968
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23406
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.157
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.016
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53492
_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_density_diffrn    1.305
_exptl_crystal_description       Block
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.112
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.2168
_refine_ls_R_factor_gt           0.0869
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1998
_refine_ls_wR_factor_ref         0.2897
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2385
_reflns_number_total             5964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03708k2.cif
_cod_data_source_block           Complex3_Y
_cod_depositor_comments
'Adding full bibliography for 7708907--7708909.cif.'
_cod_original_cell_volume        6788.7(11)
_cod_database_code               7708908
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'c100 h100 n10 o10 Si6 Gd2'
_shelx_estimated_absorpt_t_max   0.752
_shelx_estimated_absorpt_t_min   0.689
_reflns_odcompleteness_completeness 92.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.03
_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(O2) = Uanis(C22) = Uanis(C23) = Uanis(C24) = Uanis(C25)
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10)
3.b Secondary CH2 refined with riding coordinates:
 C14(H14a,H14b), C17(H17a,H17b), C13(H13a,H13b), C15(H15a,H15b), C16(H16a,
 H16b), C19(H19a,H19b), C18(H18a,H18b), C20(H20a,H20b), C25(H25a,H25b),
 C23(H23a,H23b), C24(H24a,H24b), C22(H22a,H22b)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C3(H3)
3.d Idealised Me refined as rotating group:
 C27(H27a,H27b,H27c), C26(H26a,H26b,H26c), C0AA(H0Aa,H0Ab,H0Ac), C8(H8a,H8b,
 H8c), C9(H9a,H9b,H9c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c)
;
_shelx_res_checksum              9416
_shelx_hkl_checksum              58900
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.325
_oxdiff_exptl_absorpt_empirical_full_min 0.857