Synthesis and Reactivity of Four-Membered Azapalladacycles Derived fromN,N-Dialkyl-2-iodoanilines: Insertion Reactions of Carbenes into the Carbon−Palladium Bond
Solé, Daniel; Vallverdú, Lluís; Solans, Xavier; Font-Bardia, Mercè; Bonjoch, Josep; Organometallics 23 (2004) 1438–; doi:10.1021/om034270c

data_4076258
_publ_section_title
;
 Synthesis and Reactivity of Four-Membered Azapalladacycles Derived
 fromN,N-Dialkyl-2-iodoanilines:&#x00A0; Insertion Reactions of Carbenes
 into the Carbon&#x2212;Palladium Bond
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1438
_journal_paper_doi               10.1021/om034270c
_journal_volume                  23
_journal_year                    2004
_chemical_formula_sum            'C60 H62 I2 N2 O4 P2 Pd2'
_chemical_formula_weight         1403.66
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.27
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.9350(10)
_cell_length_b                   14.3460(10)
_cell_length_c                   16.9290(10)
_cell_measurement_temperature    293(2)
_cell_volume                     2896.3(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.592
_diffrn_measured_fraction_theta_max 0.592
_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  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10477
_diffrn_reflns_theta_full        28.92
_diffrn_reflns_theta_max         28.92
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    1.788
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1392
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       0.0008(5)
_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   1.179
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1513P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2142
_refine_ls_wR_factor_ref         0.2325
_reflns_number_gt                3320
_reflns_number_total             4698
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om034270csi20040114_041317.cif
_cod_data_source_block           9a
_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 2.4.1 from 2010-06-29.

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/[\s^2^(Fo^2^)+(0.1513P)^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^)+(0.1513P)^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_original_sg_symbol_H-M      P21/n
_cod_database_code               4076258