#------------------------------------------------------------------------------
#$Date: 2016-03-21 15:08:08 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178738 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/49/4084990.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_4084990
loop_
_publ_author_name
'Koller, Stephan G.'
'Martín-Romo, Raquel'
'Melero, José S.'
'Colquhoun, Victoria P.'
'Schildbach, Daniel'
'Strohmann, Carsten'
'Villafañe, Fernando'
_publ_section_title
;
 Structural Consequences of an Extreme Difference between
 theTransInfluence of the Donor Atoms in a Palladacycle
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7329
_journal_paper_doi               10.1021/om501100y
_journal_volume                  33
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_sum            'C24 H29 N Pd Si'
_chemical_formula_weight         465.97
_chemical_name_systematic
;
    ?
;
_space_group_IT_number           92
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-12-18T15:38:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.1110(17)
_cell_length_b                   12.1110(17)
_cell_length_c                   33.215(3)
_cell_measurement_temperature    173(2)
_cell_volume                     4871.9(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            31854
_diffrn_reflns_theta_full        27
_diffrn_reflns_theta_max         27
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    0.818
_exptl_absorpt_correction_T_max  0.8534
_exptl_absorpt_correction_T_min  0.7355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'FACEIT in IPDS (Stoe & Cie, 1997)'
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.808
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.158
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.048
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1140P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1535
_reflns_number_gt                4540
_reflns_number_total             5322
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501100y_si_002.cif
_cod_data_source_block           js66c
_cod_depositor_comments
'Adding full bibliography for 4084989--4084991.cif.'
_cod_database_code               4084990
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z+3/4'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, -z+1/4'
'y, x, -z'
'y+1/2, -x+1/2, z+3/4'
'-y+1/2, x+1/2, z+1/4'
'-y, -x, -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
Pd Pd 0.41533(3) -0.07446(3) 0.020974(9) 0.03761(14) Uani 1 1 d .
Si Si 0.49075(11) 0.14492(10) 0.05882(3) 0.0309(3) Uani 1 1 d .
N N 0.4314(4) 0.0696(3) -0.01701(11) 0.0403(9) Uani 1 1 d .
C1 C 0.3907(4) 0.0333(4) 0.06868(14) 0.0354(10) Uani 1 1 d .
H1A H 0.3142 0.0619 0.0689 0.042 Uiso 1 1 calc R
H1B H 0.4061 -0.0033 0.0947 0.042 Uiso 1 1 calc R
C2 C 0.6240(4) 0.1214(5) 0.08733(15) 0.0402(10) Uani 1 1 d .
C3 C 0.6656(7) 0.1993(7) 0.1129(2) 0.078(3) Uani 1 1 d .
H3 H 0.6276 0.2674 0.1159 0.094 Uiso 1 1 calc R
C4 C 0.7629(8) 0.1815(10) 0.1348(3) 0.099(3) Uani 1 1 d .
H4 H 0.7913 0.238 0.1517 0.119 Uiso 1 1 calc R
C5 C 0.8166(6) 0.0826(8) 0.1318(2) 0.075(2) Uani 1 1 d .
H5 H 0.8789 0.0678 0.1483 0.09 Uiso 1 1 calc R
C6 C 0.7808(8) 0.0048(8) 0.1049(4) 0.101(3) Uani 1 1 d .
H6 H 0.8206 -0.0621 0.1014 0.121 Uiso 1 1 calc R
C7 C 0.6843(7) 0.0251(7) 0.0824(3) 0.086(3) Uani 1 1 d .
H7 H 0.6599 -0.0284 0.0635 0.103 Uiso 1 1 calc R
C8 C 0.4370(4) 0.2843(4) 0.07376(14) 0.0341(9) Uani 1 1 d .
C9 C 0.3732(5) 0.2945(4) 0.10828(16) 0.0462(12) Uani 1 1 d .
H9 H 0.3557 0.2304 0.1235 0.055 Uiso 1 1 calc R
C10 C 0.3340(6) 0.3981(5) 0.12124(18) 0.0521(14) Uani 1 1 d .
H10 H 0.2911 0.4031 0.1451 0.062 Uiso 1 1 calc R
C11 C 0.3572(5) 0.4915(5) 0.09965(19) 0.0476(13) Uani 1 1 d .
H11 H 0.3303 0.5611 0.1085 0.057 Uiso 1 1 calc R
C12 C 0.4198(5) 0.4843(4) 0.06511(16) 0.0427(11) Uani 1 1 d .
H12 H 0.4362 0.549 0.0501 0.051 Uiso 1 1 calc R
C13 C 0.4595(4) 0.3805(4) 0.05200(15) 0.0363(10) Uani 1 1 d .
H13 H 0.5022 0.3761 0.0281 0.044 Uiso 1 1 calc R
C14 C 0.5199(5) 0.1368(4) 0.00311(14) 0.0392(10) Uani 1 1 d .
H14A H 0.5215 0.212 -0.0085 0.047 Uiso 1 1 calc R
H14B H 0.5929 0.1021 -0.0014 0.047 Uiso 1 1 calc R
C15 C 0.3306(5) 0.1364(4) -0.01926(16) 0.0446(12) Uani 1 1 d .
H15A H 0.3463 0.2049 -0.0345 0.053 Uiso 1 1 calc R
H15B H 0.3079 0.1577 0.0083 0.053 Uiso 1 1 calc R
C16 C 0.2352(6) 0.0746(6) -0.03972(18) 0.0586(15) Uani 1 1 d .
H16A H 0.2169 0.0074 -0.0242 0.07 Uiso 1 1 calc R
H16B H 0.1689 0.1223 -0.0405 0.07 Uiso 1 1 calc R
C17 C 0.2682(7) 0.0435(6) -0.08164(18) 0.067(2) Uani 1 1 d .
H17A H 0.2769 0.111 -0.0981 0.08 Uiso 1 1 calc R
H17B H 0.2096 -0.0023 -0.094 0.08 Uiso 1 1 calc R
C18 C 0.3764(7) -0.0206(6) -0.08119(17) 0.067(2) Uani 1 1 d .
H18A H 0.3638 -0.0934 -0.0684 0.08 Uiso 1 1 calc R
H18B H 0.4005 -0.0337 -0.1093 0.08 Uiso 1 1 calc R
C19 C 0.4663(6) 0.0386(5) -0.05897(15) 0.0532(15) Uani 1 1 d .
H19A H 0.4868 0.1062 -0.074 0.064 Uiso 1 1 calc R
H19B H 0.5323 -0.0095 -0.0576 0.064 Uiso 1 1 calc R
C20 C 0.3448(8) -0.2550(5) -0.0057(2) 0.0670(19) Uani 1 1 d .
H20 H 0.2902 -0.2656 -0.0259 0.08 Uiso 1 1 calc R
C21 C 0.3259(8) -0.2421(5) 0.0353(2) 0.070(2) Uani 1 1 d .
H21 H 0.2554 -0.2435 0.0479 0.084 Uiso 1 1 calc R
C22 C 0.4217(10) -0.2275(4) 0.05453(17) 0.077(3) Uani 1 1 d .
H22 H 0.4302 -0.211 0.0823 0.092 Uiso 1 1 calc R
C23 C 0.5081(7) -0.2409(5) 0.0264(2) 0.067(2) Uani 1 1 d .
H23 H 0.5849 -0.2436 0.0321 0.081 Uiso 1 1 calc R
C24 C 0.4577(7) -0.2495(5) -0.0118(2) 0.067(2) Uani 1 1 d .
H24 H 0.4946 -0.2512 -0.037 0.08 Uiso 1 1 calc R
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'
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 '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
C1 Pd N 87.20(17)
C1 Si C8 112.6(2)
C1 Si C14 105.0(2)
C8 Si C14 111.8(2)
C1 Si C2 111.1(2)
C8 Si C2 107.4(2)
C14 Si C2 108.9(2)
C15 N C19 108.9(4)
C15 N C14 108.6(4)
C19 N C14 110.3(4)
C15 N Pd 113.5(3)
C19 N Pd 111.4(3)
C14 N Pd 104.0(3)
Si C1 Pd 103.4(2)
C3 C2 C7 117.4(6)
C3 C2 Si 121.5(5)
C7 C2 Si 121.1(5)
C2 C3 C4 121.8(8)
C5 C4 C3 119.8(9)
C6 C5 C4 120.1(7)
C5 C6 C7 119.2(8)
C2 C7 C6 121.5(8)
C9 C8 C13 117.5(5)
C9 C8 Si 119.5(4)
C13 C8 Si 123.0(4)
C8 C9 C10 121.3(5)
C11 C10 C9 120.5(5)
C10 C11 C12 119.8(5)
C11 C12 C13 120.0(5)
C8 C13 C12 121.0(5)
N C14 Si 109.3(3)
N C15 C16 112.4(5)
C17 C16 C15 109.5(6)
C16 C17 C18 110.4(5)
C19 C18 C17 112.7(6)
C18 C19 N 111.8(5)
C24 C20 C21 107.5(8)
C22 C21 C20 109.8(8)
C21 C22 C23 108.2(6)
C24 C23 C22 106.4(7)
C20 C24 C23 107.4(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd C1 2.074(5)
Pd N 2.162(4)
Si C1 1.845(5)
Si C8 1.876(5)
Si C14 1.886(5)
Si C2 1.893(5)
N C15 1.467(7)
N C19 1.504(6)
N C14 1.502(7)
C2 C3 1.366(9)
C2 C7 1.385(9)
C3 C4 1.401(10)
C4 C5 1.367(14)
C5 C6 1.368(15)
C6 C7 1.409(11)
C8 C9 1.388(7)
C8 C13 1.398(7)
C9 C10 1.409(8)
C10 C11 1.369(9)
C11 C12 1.377(9)
C12 C13 1.415(7)
C15 C16 1.535(8)
C16 C17 1.497(9)
C17 C18 1.522(12)
C18 C19 1.498(10)
C20 C24 1.383(12)
C20 C21 1.392(10)
C21 C22 1.336(13)
C22 C23 1.412(12)
C23 C24 1.412(11)
