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_7708907
_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 Gd2 Li2 N2 O6 Si2'
_chemical_formula_sum            'C54 H100 Cl6 Gd2 Li2 N2 O6 Si2'
_chemical_formula_weight         1470.61
_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             2021-04-27
_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                   18.9685(3)
_cell_length_b                   17.2945(3)
_cell_length_c                   20.8481(5)
_cell_measurement_reflns_used    7768
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      27.3860
_cell_measurement_theta_min      1.9200
_cell_volume                     6839.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_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     -6.56 100.24   0.60    2.00    --    9.89  30.17-131.81  178
  2  \f    -34.56 126.24   0.60    2.00  81.02  -9.84  31.50    --   268
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0023894000
_diffrn_orient_matrix_UB_12      -0.0366540000
_diffrn_orient_matrix_UB_13      0.0151251000
_diffrn_orient_matrix_UB_21      -0.0313965000
_diffrn_orient_matrix_UB_22      -0.0079104000
_diffrn_orient_matrix_UB_23      -0.0172629000
_diffrn_orient_matrix_UB_31      0.0201683000
_diffrn_orient_matrix_UB_32      -0.0166323000
_diffrn_orient_matrix_UB_33      -0.0251069000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0348
_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            46826
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         2.147
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.235
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    1.428
_exptl_crystal_description       block
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.754
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         6019
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0046P)^2^+50.7012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.1002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4212
_reflns_number_total             6019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03708k2.cif
_cod_data_source_block           Complex1_Gd
_cod_depositor_comments
'Adding full bibliography for 7708907--7708909.cif.'
_cod_database_code               7708907
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Li Si Cl Gd'
_reflns_odcompleteness_completeness 87.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.73
_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(C42) = Uanis(C45) = Uanis(C44) = Uanis(C43)
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10)
3.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C35(H35A,
 H35B), C32(H32A,H32B), C34(H34A,H34B), C33(H33A,H33B), C44(H44A,H44B),
 C43(H43A,H43B), C45(H45A,H45B), C42(H42A,H42B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5)
3.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C8(H8A,H8B,H8C), C15(H15A,H15B,H15C), C9(H9A,H9B,H9C),
 C14(H14A,H14B,H14C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              42736
_shelx_hkl_checksum              85857
_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 1.367
_oxdiff_exptl_absorpt_empirical_full_min 0.751