Molecular and electronic structure of the dithiooxalato radical ligand stabilised by rare earth coordination.
McGuire, Jake; Wilson, Bradley; McAllister, James; Miras, Haralampos N.; Wilson, Claire; Sproules, Stephen; Farnaby, Joy H.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 5491–5495; doi:10.1039/c9dt00688e

data_7049331
_publ_section_title
;
 Molecular and electronic structure of the dithiooxalato radical ligand
 stabilised by rare earth coordination.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5491
_journal_page_last               5495
_journal_paper_doi               10.1039/c9dt00688e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C40 H40 B4 Gd2 N24 Ni O4 S4, 2(C H2 Cl2)'
_chemical_formula_sum            'C42 H44 B4 Cl4 Gd2 N24 Ni O4 S4'
_chemical_formula_weight         1635.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-02-14 deposited with the CCDC.    2019-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                79.546(3)
_cell_angle_beta                 86.774(3)
_cell_angle_gamma                72.601(3)
_cell_formula_units_Z            1
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_cell_length_b                   11.475(2)
_cell_length_c                   17.902(4)
_cell_measurement_reflns_used    5239
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.220
_cell_measurement_theta_min      2.313
_cell_volume                     1494.7(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Diamond3
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Apex II Quazar CCD'
_diffrn_measurement_method       '\w & \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16210
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.637
_diffrn_reflns_theta_min         1.888
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.887
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6664
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_description       plates
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.453
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         6264
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0208P)^2^+1.7373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0633
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5327
_reflns_number_total             6264
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00688e2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7049330--7049334.cif.'
_cod_database_code               7049331
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.761
_shelx_estimated_absorpt_t_max   0.945
_shelx_res_checksum              49563