Convenient Synthetic Route to Palladium Complexes of Unconventional N-Heterocyclic Carbenes Derived from Pyridazine and Phthalazine
Guo, Tongxun; Dechert, Sebastian; Meyer, Steffen; Meyer, Franc; Organometallics 31 (2012) 8537–; doi:10.1021/om300899r

data_4079637
_publ_section_title
;
 Convenient Synthetic Route to Palladium Complexes of Unconventional
 N-Heterocyclic Carbenes Derived from Pyridazine and Phthalazine
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              8537
_journal_paper_doi               10.1021/om300899r
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C47 H44 Cl N4 P2 Pd +, B F4 -, C H2 Cl2'
_chemical_formula_sum            'C48 H46 B Cl3 F4 N4 P2 Pd'
_chemical_formula_weight         1040.39
_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                 97.243(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.2960(5)
_cell_length_b                   10.4914(2)
_cell_length_c                   32.2000(12)
_cell_measurement_reflns_used    45238
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      1.27
_cell_volume                     4791.0(3)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       \w
_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  0.0929
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            45238
_diffrn_reflns_theta_full        25.69
_diffrn_reflns_theta_max         25.69
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_T_max  0.9608
_exptl_absorpt_correction_T_min  0.8053
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.173
_refine_diff_density_min         -1.519
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       0.0019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         9032
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0819P)^2^+3.6783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1437
_reflns_number_gt                7334
_reflns_number_total             9032
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300899r_si_002.cif
_cod_data_source_block           4-togu22
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4079637