From NHC to Imidazolyl Ligand: Synthesis of Platinum and Palladium Complexes d10-[M(NHC)2] (M = Pd, Pt) of the NHC 1,3-Diisopropylimidazolin-2-ylidene
Hering, Florian; Radius, Udo; Organometallics 34 (2015) 3236–; doi:10.1021/acs.organomet.5b00277

data_4086175
_publ_section_title
;
 From NHC to Imidazolyl Ligand: Synthesis of Platinum and Palladium
 Complexes d10-[M(NHC)2] (M = Pd, Pt) of the NHC
 1,3-Diisopropylimidazolin-2-ylidene
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3236
_journal_paper_doi               10.1021/acs.organomet.5b00277
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C18 H32 Cl2 N4 Pt'
_chemical_formula_weight         570.46
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6775(8)
_cell_length_b                   13.0430(12)
_cell_length_c                   18.9916(18)
_cell_measurement_reflns_used    9431
_cell_measurement_temperature    168(2)
_cell_measurement_theta_max      26.07
_cell_measurement_theta_min      2.65
_cell_volume                     2149.5(3)
_computing_cell_refinement       'Saint+ ver. 7.68A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2010.3 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.68A (Bruker AXS)'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      168(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            48275
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.198
_diffrn_reflns_theta_min         1.894
_exptl_absorpt_coefficient_mu    6.785
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.29
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'SadAbs-2008/1 (Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 1802 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.003(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         4304
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0137
_refine_ls_R_factor_gt           0.0134
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0148P)^2^+0.1030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0325
_refine_ls_wR_factor_ref         0.0326
_reflns_Friedel_coverage         0.750
_reflns_friedel_fraction_full    0.997
_reflns_friedel_fraction_max     0.994
_reflns_number_gt                4260
_reflns_number_total             4304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00277_si_003.cif
_cod_data_source_block           compound_cis-10
_cod_database_code               4086175
_shelx_estimated_absorpt_t_min   0.172
_shelx_estimated_absorpt_t_max   0.522
_shelxl_version_number           2013-4
_shelx_res_checksum              21755
_shelx_hkl_checksum              75824