Towards New Coordination Modes of 1,2,3-Triazolylidene: Controlled by the Nature of 1st Metalation in a Heteroditopic Bis-NHC Ligand
Rit, Arnab; Illam, Praseetha Mathoor; Tiwari, Chandra Shekhar; Chemical Science  (2022) –; doi:10.1039/D2SC05024B

data_1567822
_publ_section_title
;
 Towards New Coordination Modes of 1,2,3-Triazolylidene: Controlled by the
 Nature of 1st Metalation in a Heteroditopic Bis-NHC Ligand
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC05024B
_journal_year                    2022
_chemical_formula_moiety         'C20 H23 Br2 N6 Pd, Br [+ solvent]'
_chemical_formula_sum            'C20 H23 Br3 N6 Pd'
_chemical_formula_weight         693.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-05-31 deposited with the CCDC.	2022-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.656(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.5000(9)
_cell_length_b                   11.2281(5)
_cell_length_c                   23.8483(10)
_cell_measurement_reflns_used    3785
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.44
_cell_measurement_theta_min      2.63
_cell_volume                     5186.3(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa Apex2 CCD'
_diffrn_measurement_method       '\w and \f sacn'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15547
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.946
_diffrn_reflns_theta_max         24.946
_diffrn_reflns_theta_min         1.719
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    5.356
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.4928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (BRuker)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_description       BLock
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4548
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0431P)^2^+4.5068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0923
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3251
_reflns_number_total             4548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc05024b2.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1567822
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.414
_shelx_estimated_absorpt_t_max   0.616
_shelx_res_checksum              62678
_shelx_hkl_checksum              65668
_shelx_fab_checksum              61149