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_7049333
_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         'C4 Cl8 Ni O4 S4 Sn2, 2(C24 H20 P)'
_chemical_formula_sum            'C52 H40 Cl8 Ni O4 P2 S4 Sn2'
_chemical_formula_weight         1498.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-19
_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                 90.339(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.5323(4)
_cell_length_b                   21.6051(13)
_cell_length_c                   17.9843(10)
_cell_measurement_reflns_used    9095
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.20
_cell_volume                     2926.6(3)
_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  'XL (Sheldrick, 2008)'
_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 0.997
_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  0.0465
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36852
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.310
_diffrn_reflns_theta_min         2.199
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.771
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0872 before and 0.0679 after correction. The Ratio of minimum to maximum transmission is 0.8849. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_description       lath
_exptl_crystal_F_000             1484
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         7242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+2.8407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0738
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5969
_reflns_number_total             7242
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00688e2.cif
_cod_data_source_block           PPh42Nidto2Sn2Cl8
_cod_depositor_comments
'Adding full bibliography for 7049330--7049334.cif.'
_cod_database_code               7049333
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.523
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2P(H2P), C3P(H3P), C4P(H4P), C5P(H5P), C6P(H6P), C8P(H8P), C9P(H9P),
 C10P(H10P), C11P(H11P), C12P(H12P), C14P(H14P), C15P(H15P), C16P(H16P),
 C17P(H17P), C18P(H18P), C20P(H20P), C21P(H21P), C22P(H22P), C23P(H23P),
 C24P(H24P)
;
_shelx_res_checksum              46945
_olex2_submission_special_instructions 'No special instructions were received'