Activation of the C-N Bond in Nitromethane by Palladium α-Diimine Complexes
Suzanne R. Golisz; Nilay Hazari; Jay A. Labinger; John E. Bercaw; Journal of Organic Chemistry 74 (2009) 8441–8443; doi:10.1021/jo901635g

data_4024951
_publ_contact_author
;
 Dr J. Bercaw or Dr J. Labinger           
 Arnold and Mabel Beckman Laboratories of Chemical Synthesis, 
 California Institute of Technology, 
 Pasadena, California 91125
;
_publ_contact_author_email       'bercaw@caltech.edu or jal@caltech.edu'
_publ_contact_author_fax         '+1 1865 285141'
_publ_contact_author_phone       '+1 626 395 6576'
_publ_section_title
;
Activation of the C-N Bond in Nitromethane by Palladium \a-Diimine
Complexes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8441
_journal_page_last               8443
_journal_paper_doi               10.1021/jo901635g
_journal_volume                  74
_journal_year                    2009
_chemical_formula_moiety         'C16 H28 N4 O4 Pd, 0.5(C3 H6 O)'
_chemical_formula_sum            'C17.5 H31 N4 O4.5 Pd'
_chemical_formula_weight         475.86
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.1919(5)
_cell_length_b                   13.4354(6)
_cell_length_c                   25.0193(11)
_cell_measurement_reflns_used    9739
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.60
_cell_measurement_theta_min      2.33
_cell_volume                     4098.2(3)
_computing_cell_refinement       'Bruker SAINT-Plus v7.34A'
_computing_data_collection       'Bruker APEX2 v2.1-0'
_computing_data_reduction        'Bruker SAINT-Plus v7.34A'
_computing_molecular_graphics    'Bruker XP v5.1'
_computing_publication_material  'Bruker XCIF 2008'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w scans; 15 settings'
_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  0.0934
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            99109
_diffrn_reflns_theta_full        35.27
_diffrn_reflns_theta_max         35.27
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.938
_exptl_absorpt_correction_T_max  0.8799
_exptl_absorpt_correction_T_min  0.7925
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Fragment
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.144
_refine_diff_density_min         -0.993
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.106
_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     266
_refine_ls_number_reflns         8513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.106
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/s^2^(Fo^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0700
_reflns_number_gt                6502
_reflns_number_total             8513
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo901635g_si_002_2.cif
_cod_data_source_block           COMPOUND_1b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_refine_ls_weighting_scheme' value 'Sigma' changed to
'sigma' 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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct methods' was changed to
'direct'.

'_atom_sites_solution_secondary' value 'Difference Fourier map' was
changed to 'difmap'.

'_atom_sites_solution_hydrogens' value 'Geometric positions' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      Pbcn
_cod_original_formula_sum        'C17.50 H31 N4 O4.50 Pd'
_cod_database_code               4024951