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_7049334
_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, C10 H10 Co, C2 H3 N'
_chemical_formula_sum            'C52 H53 B4 Co Gd2 N25 Ni O4 S4'
_chemical_formula_weight         1695.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-20 deposited with the CCDC.    2019-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.674(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5505(14)
_cell_length_b                   18.3268(9)
_cell_length_c                   18.0741(11)
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.20
_cell_volume                     6537.7(7)
_computing_cell_refinement       'SAINT V8.37A (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'charge integrating pixel array detector'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            67695
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.322
_diffrn_reflns_theta_min         2.198
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.728
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1009 before and 0.0692 after correction. The Ratio of minimum to maximum transmission is 0.8050. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_description       plate
_exptl_crystal_F_000             3356
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.492
_refine_diff_density_min         -1.398
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         16204
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0455P)^2^+12.9133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.1069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11900
_reflns_number_total             16204
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00688e2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7049330--7049334.cif.'
_cod_database_code               7049334
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.585
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1T(H1TA), B2T(H2TA), B3T(H3TA), B4T(H4TA)
2.b Aromatic/amide H refined with riding coordinates:
 C1T(H1T), C2T(H2T), C3T(H3T), C4T(H4T), C5T(H5T), C6T(H6T), C7T(H7T),
 C8T(H8T), C9T(H9T), C10T(H10T), C11T(H11T), C12T(H12T), C13T(H13T), C14T(H14T),
  C15T(H15T), C16T(H16T), C17T(H17T), C18T(H18T), C19T(H19T), C20T(H20T),
 C21T(H21T), C22T(H22T), C23T(H23T), C24T(H24T), C25T(H25T), C26T(H26T),
 C27T(H27T), C28T(H28T), C29T(H29T), C30T(H30T), C31T(H31T), C32T(H32T),
 C33T(H33T), C34T(H34T), C35T(H35T), C36T(H36T), C1C(H1C), C2C(H2C), C3C(H3C),
 C4C(H4C), C5C(H5C), C6C(H6C), C7C(H7C), C8C(H8C), C9C(H9C), C10C(H10C)
2.c Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC)
;
_shelx_res_checksum              45980
_olex2_submission_special_instructions 'No special instructions were received'