#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:47:24 +0100 (vie 25 de mar de 2016) $
#$Revision: 179764 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/60/7006027.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7006027
loop_
_publ_author_name
'Solé, Daniel'
'Solans, Xavier'
'Font-Bardia, Mercé'
_publ_section_title
;
 N,N-Dialkyl-2-iodoanilines: a versatile source for the synthesis of
 Pd(ii) complexes. Synthesis of novel OCP- and CCN-pincer palladium
 complexes.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4286
_journal_page_last               4292
_journal_paper_doi               10.1039/b708306h
_journal_year                    2007
_chemical_formula_sum            'C24 H32 N4 O2 Pd2'
_chemical_formula_weight         621.34
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            4
_cell_length_a                   7.688(5)
_cell_length_b                   11.928(7)
_cell_length_c                   25.540(8)
_cell_measurement_reflns_used    1112
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31
_cell_measurement_theta_min      3
_cell_volume                     2342(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.587
_diffrn_measured_fraction_theta_max 0.587
_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  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0835
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1741
_diffrn_reflns_theta_full        28.51
_diffrn_reflns_theta_max         28.51
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    1.564
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.893
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.219
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1741
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.225
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0839P)²+1.1933P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1407
_reflns_number_gt                1606
_reflns_number_total             1741
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b708306h.txt
_cod_data_source_block           sokm21c
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7006027
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.44612(4) 0.47653(2) 0.574268(12) 0.0387(2) Uani 1 1 d U . .
N1 N 0.7164(4) 0.3189(3) 0.55770(16) 0.0469(7) Uani 1 1 d . . .
N2 N 0.2279(5) 0.5336(3) 0.62213(16) 0.0489(8) Uani 1 1 d U . .
O O 0.6674(4) 0.4211(3) 0.48711(13) 0.0519(7) Uani 1 1 d . . .
C1 C 0.8408(6) 0.2459(4) 0.52946(18) 0.0536(10) Uani 1 1 d . . .
H1A H 0.8488 0.2695 0.4936 0.080 Uiso 1 1 calc R . .
H1B H 0.8011 0.1697 0.5309 0.080 Uiso 1 1 calc R . .
H1C H 0.9533 0.2513 0.5456 0.080 Uiso 1 1 calc R . .
C2 C 0.6777(5) 0.3066(4) 0.61012(18) 0.0507(9) Uani 1 1 d . . .
C3 C 0.7543(6) 0.2279(4) 0.6439(2) 0.0605(12) Uani 1 1 d . . .
H3 H 0.8346 0.1764 0.6311 0.073 Uiso 1 1 calc R . .
C4 C 0.7085(6) 0.2275(4) 0.6973(2) 0.0619(12) Uani 1 1 d . . .
H4 H 0.7580 0.1750 0.7197 0.074 Uiso 1 1 calc R . .
C5 C 0.5913(6) 0.3042(5) 0.7165(2) 0.0600(11) Uani 1 1 d . . .
H5 H 0.5592 0.3029 0.7516 0.072 Uiso 1 1 calc R . .
C6 C 0.5179(6) 0.3876(4) 0.68113(18) 0.0522(9) Uani 1 1 d U . .
C7 C 0.5535(5) 0.3886(4) 0.62526(19) 0.0489(10) Uani 1 1 d U . .
C8 C 0.3916(9) 0.4703(5) 0.7004(3) 0.0735(14) Uani 1 1 d U . .
H8A H 0.4444 0.5440 0.6986 0.088 Uiso 1 1 calc R . .
H8B H 0.3678 0.4544 0.7369 0.088 Uiso 1 1 calc R . .
C9 C 0.2213(7) 0.4738(4) 0.67126(18) 0.0533(11) Uani 1 1 d . . .
H9A H 0.1837 0.3975 0.6646 0.064 Uiso 1 1 calc R . .
H9B H 0.1346 0.5088 0.6935 0.064 Uiso 1 1 calc R . .
C10 C 0.0683(7) 0.5107(6) 0.5909(4) 0.0737(17) Uani 1 1 d . . .
H10A H 0.0742 0.5510 0.5584 0.111 Uiso 1 1 calc R . .
H10B H -0.0322 0.5346 0.6102 0.111 Uiso 1 1 calc R . .
H10C H 0.0601 0.4318 0.5839 0.111 Uiso 1 1 calc R . .
C11 C 0.2397(6) 0.6561(4) 0.6306(2) 0.0589(10) Uani 1 1 d . . .
H11A H 0.2464 0.6936 0.5974 0.088 Uiso 1 1 calc R . .
H11B H 0.3419 0.6728 0.6508 0.088 Uiso 1 1 calc R . .
H11C H 0.1385 0.6814 0.6492 0.088 Uiso 1 1 calc R . .
C12 C 0.6293(5) 0.4043(3) 0.52995(16) 0.0442(8) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 Pd C12 80.87(19) . . ?
C7 Pd O 177.31(15) . 5_666 ?
C12 Pd O 96.70(14) . 5_666 ?
C7 Pd N2 97.14(17) . . ?
C12 Pd N2 172.24(14) . . ?
O Pd N2 85.41(13) 5_666 . ?
C2 N1 C12 117.6(3) . . ?
C2 N1 C1 123.3(4) . . ?
C12 N1 C1 119.1(4) . . ?
C9 N2 C11 111.2(4) . . ?
C9 N2 C10 110.3(5) . . ?
C11 N2 C10 108.1(4) . . ?
C9 N2 Pd 111.1(3) . . ?
C11 N2 Pd 110.0(3) . . ?
C10 N2 Pd 106.0(4) . . ?
C12 O Pd 133.0(3) . 5_666 ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 125.3(4) . . ?
N1 C2 C7 109.6(4) . . ?
C3 C2 C7 125.1(5) . . ?
C2 C3 C4 119.5(5) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 120.5(5) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 119.2(5) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C7 C6 C5 122.7(5) . . ?
C7 C6 C8 116.6(5) . . ?
C5 C6 C8 120.5(5) . . ?
C2 C7 C6 112.9(4) . . ?
C2 C7 Pd 119.7(4) . . ?
C6 C7 Pd 127.4(3) . . ?
C6 C8 C9 115.4(5) . . ?
C6 C8 H8A 108.4 . . ?
C9 C8 H8A 108.4 . . ?
C6 C8 H8B 108.4 . . ?
C9 C8 H8B 108.4 . . ?
H8A C8 H8B 107.5 . . ?
N2 C9 C8 114.3(4) . . ?
N2 C9 H9A 108.7 . . ?
C8 C9 H9A 108.7 . . ?
N2 C9 H9B 108.7 . . ?
C8 C9 H9B 108.7 . . ?
H9A C9 H9B 107.6 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O C12 N1 118.9(4) . . ?
O C12 Pd 130.0(3) . . ?
N1 C12 Pd 111.1(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd C7 1.865(5) . ?
Pd C12 2.002(4) . ?
Pd O 2.171(3) 5_666 ?
Pd N2 2.184(4) . ?
N1 C2 1.379(5) . ?
N1 C12 1.410(5) . ?
N1 C1 1.481(5) . ?
N2 C9 1.444(5) . ?
N2 C11 1.481(6) . ?
N2 C10 1.489(8) . ?
O C12 1.150(5) . ?
O Pd 2.171(3) 5_666 ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.404(6) . ?
C2 C7 1.421(6) . ?
C3 C4 1.408(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.374(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.457(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.453(6) . ?
C6 C8 1.468(8) . ?
C8 C9 1.506(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
