Synthesis of Novel Phosphaalkene-Based Bidentate Ligands Mes*PCH(3-R-Ar) (R = Pyridyl, Carbaldimino) and Formation of Three-Membered Palladacycles Mes*(Me)P−CH(3-R-Ar)−PdCl by Carbapalladation of the PC Double Bond†
van der Sluis, Marcel; Beverwijk, Vincent; Termaten, Arjan; Bickelhaupt, Friedrich; Kooijman, Huub; Spek, Anthony L.; Organometallics 18 (1999) 1402–; doi:10.1021/om980913q

data_4077748
_publ_section_title
;
 Synthesis of Novel Phosphaalkene-Based Bidentate Ligands Mes*PCH(3-R-Ar)
 (R = Pyridyl, Carbaldimino) and Formation of Three-Membered Palladacycles
 Mes*(Me)P&#x2212;CH(3-R-Ar)&#x2212;PdCl by Carbapalladation of the PC
 Double Bond&#x2020;
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1402
_journal_paper_doi               10.1021/om980913q
_journal_volume                  18
_journal_year                    1999
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C62 H82 Cl2 N2 P2 Pd2, 8(C H Cl3)'
_chemical_formula_sum            'C70 H90 Cl26 N2 P2 Pd2'
_chemical_formula_weight         2155.92
_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'
_cell_angle_alpha                90
_cell_angle_beta                 97.998(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6333(17)
_cell_length_b                   18.674(3)
_cell_length_c                   18.330(3)
_cell_measurement_temperature    150
_cell_volume                     4621.2(12)
_computing_cell_refinement       'SET4 (de Boer & Duisenberg, 1984)'
_computing_data_collection       'Locally modified CAD4-Version 5 Software'
_computing_data_reduction        'HELENA (Spek, 1997)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1081
_diffrn_reflns_av_sigmaI/netI    0.1618
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16009
_diffrn_reflns_reduction_process
;
 ?
;
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    1.21
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             2176
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    'H-atom refinement: see text '
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         8142
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1519
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/[\
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1450
_reflns_number_gt                4313
_reflns_number_total             8142
_reflns_threshold_expression     >2sigma(i)
_cod_data_source_file            om980913q.cif
_cod_data_source_block           s1532b
_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 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[\' was changed to
'calc'. New tag '_refine_ls_weighting_details' was created. The value
of the new tag was set to 'w=1/[\'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4077748