Synthesis of Complexes with Protic NH,NH-NHC Ligands via Oxidative Addition of 2-Halogenoazoles to Zero-Valent Transition Metals
Das, Rajorshi; Hepp, Alexander; Daniliuc, Constantin G.; Hahn, F. Ekkehardt; Organometallics 33 (2014) 6975–; doi:10.1021/om501120u

data_4084861
_publ_section_title
;
 Synthesis of Complexes with Protic NH,NH-NHC Ligands via Oxidative
 Addition of 2-Halogenoazoles to Zero-Valent Transition Metals
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6975
_journal_paper_doi               10.1021/om501120u
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C44 H38 B Cl2 F4 I N2 P2 Pd'
_chemical_formula_weight         1047.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.4550(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.6215(3)
_cell_length_b                   11.85270(10)
_cell_length_c                   18.7279(3)
_cell_measurement_reflns_used    8472
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      4.08
_cell_volume                     4268.75(10)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Montel mirror'
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            25379
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         4.09
_exptl_absorpt_coefficient_mu    1.410
_exptl_absorpt_correction_T_max  0.9723
_exptl_absorpt_correction_T_min  0.7657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.835
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         8562
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+14.6948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1145
_reflns_number_gt                7631
_reflns_number_total             8562
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501120u_si_002.cif
_cod_data_source_block           dan7348
_cod_depositor_comments
'Adding full bibliography for 4084858--4084863.cif.'
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4084861