Synthesis and Coordination Behaviour of 1H-1,2,3-Triazole-4,5-Dithiolates
Schallenberg, David; Pardemann, Nils; Villinger, Alexander; Seidel, Wolfram Willy; Dalton Transactions  (2022) –; doi:10.1039/D2DT00410K

data_7711007
_publ_section_title
;
 Synthesis and Coordination Behaviour of 1H-1,2,3-Triazole-4,5-Dithiolates
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00410K
_journal_year                    2022
_chemical_formula_moiety         'C35 H31 N3 Ni P2 S2, C H2 Cl2'
_chemical_formula_sum            'C36 H33 Cl2 N3 Ni P2 S2'
_chemical_formula_weight         763.32
_chemical_name_systematic
'[(1,2-Bis(diphenylphosphino)ethane)(1-benzyl-1H-1,2,3-triazole-4,5-dithiolato)nickel(II)]'
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-01-28 deposited with the CCDC.	2022-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.336(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9178(4)
_cell_length_b                   16.9500(7)
_cell_length_c                   20.6572(9)
_cell_measurement_reflns_used    7199
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.07
_cell_measurement_theta_min      2.40
_cell_volume                     3451.4(2)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker-Nonius Apex-X8-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            42838
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.998
_diffrn_reflns_theta_min         1.558
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.962
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       plate
_exptl_crystal_F_000             1576
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane / n-pentane'
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.030
_platon_squeeze_details
;
The unit cell contains four dichloromethane molecules which have been treated 
as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON. These were removed from the model, but included 
in the empirical formula.
;
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         9095
_refine_ls_number_restraints     325
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0656P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1334
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5555
_reflns_number_total             9095
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00410k2.cif
_cod_data_source_block           is_schal258a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7711007
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.671
_shelx_estimated_absorpt_t_max   0.972
_shelx_res_checksum              16915
_shelx_hkl_checksum              41752