Synthesis and Solid State and Solution Characterization of Mono- and Di-(η1-C) Carbamoyl−Palladium Complexes. New Efficient Palladium-Catalyzed Routes to Carbamoyl Chlorides: Key Intermediates to Isocyanates, Carbamic Esters, and Ureas
Aresta, Michele; Giannoccaro, Potenzo; Tommasi, Immacolata; Dibenedetto, Angela; Manotti Lanfredi, Anna Maria; Ugozzoli, Franco; Organometallics 19 (2000) 3879–; doi:10.1021/om000198w

data_4077507
_publ_section_title
;
 Synthesis and Solid State and Solution Characterization of Mono- and
 Di-(\h1-C) Carbamoyl&#x2212;Palladium Complexes. New Efficient
 Palladium-Catalyzed Routes to Carbamoyl Chlorides:&#x00A0; Key
 Intermediates to Isocyanates, Carbamic Esters, and Ureas
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              3879
_journal_paper_doi               10.1021/om000198w
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C22 H28 N4 O2 Pd'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   16.089(5)
_cell_length_b                   16.576(5)
_cell_length_c                   8.216(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2191.1(16)
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1093
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1826
_diffrn_reflns_theta_max         24.02
_diffrn_reflns_theta_min         3.53
_exptl_absorpt_coefficient_mu    0.871
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_F_000             1000
_refine_diff_density_max         1.680
_refine_diff_density_min         -1.322
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_coef       0.0002(12)
_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_all   0.850
_refine_ls_goodness_of_fit_obs   1.206
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         1826
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.849
_refine_ls_restrained_S_obs      1.205
_refine_ls_R_factor_all          0.1246
_refine_ls_R_factor_obs          0.0661
_refine_ls_shift/esd_max         0.038
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1282P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1797
_refine_ls_wR_factor_obs         0.1586
_reflns_number_observed          858
_reflns_number_total             1826
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om000198w.cif
_cod_data_source_block           are02
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1282P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1282P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4077507
_chemical_formula_weightical     486.88