#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/32/4083214.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_4083214
loop_
_publ_author_name
'Wahlicht, Sven'
'Brendler, Erica'
'Heine, Thomas'
'Zhechkov, Lyuben'
'Wagler, Jörg'
_publ_section_title
;
 7-Azaindol-1-yl(organo)silanes and Their PdCl2Complexes: Pd-Capped
 Tetrahedral Silicon Coordination Spheres and Paddlewheels with a Pd--Si
 Axis
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2479
_journal_paper_doi               10.1021/om401220m
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C28 H20 Cl2 N8 Pd Si'
_chemical_formula_sum            'C28 H20 Cl2 N8 Pd Si'
_chemical_formula_weight         673.91
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_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            2
_cell_length_a                   8.9934(8)
_cell_length_b                   8.9934(8)
_cell_length_c                   16.093(2)
_cell_measurement_reflns_used    2525
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.80
_cell_measurement_theta_min      2.53
_cell_volume                     1301.6(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe IPDS-2T'
_diffrn_measurement_method       'omega scans'
_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  0.0812
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3515
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    1.001
_exptl_absorpt_correction_T_max  0.9776
_exptl_absorpt_correction_T_min  0.8748
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XShape
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         602
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0331P)²+2.9894P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0994
_reflns_number_gt                485
_reflns_number_total             602
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401220m_si_002.cif
_cod_data_source_block           paddlewheel
_cod_depositor_comments
'Adding full bibliography for 4083204--4083216.cif.'
_cod_original_sg_symbol_Hall     -I4
_cod_original_sg_symbol_H-M      I4/m
_cod_database_code               4083214
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+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
Pd1 Pd 1.0000 1.0000 0.93350(14) 0.0300(5) Uani 0.50 4 d SPU . .
Si1 Si 1.0000 1.0000 1.0976(5) 0.058(4) Uani 0.50 4 d SPU . .
Cl1 Cl 1.0000 1.0000 0.7645(8) 0.099(4) Uani 0.50 4 d SP . .
Cl2 Cl 1.0000 1.0000 1.2242(13) 0.186(12) Uani 0.50 4 d SPU . .
N1 N 0.9128(19) 0.8079(17) 1.0889(6) 0.043(3) Uani 0.50 1 d PU . -1
C1 C 0.864(3) 0.710(2) 1.1521(11) 0.090(5) Uani 0.50 1 d PDU A -1
H1 H 0.8664 0.7297 1.2101 0.108 Uiso 0.50 1 calc PR A -1
C2 C 0.813(4) 0.581(3) 1.1147(9) 0.128(7) Uani 0.50 1 d PDU A -1
H2 H 0.7751 0.4967 1.1434 0.153 Uiso 0.50 1 calc PR A -1
N2 N 0.9214(18) 0.7912(14) 0.9432(8) 0.040(3) Uani 0.50 1 d PU . -1
C7 C 0.8931(11) 0.7362(10) 1.0161(8) 0.045(2) Uani 0.50 1 d PU A -1
C3 C 0.8268(10) 0.5931(10) 1.0293(9) 0.081(3) Uani 0.50 1 d PDU A -1
C4 C 0.7949(14) 0.5122(13) 0.9608(12) 0.113(4) Uani 0.50 1 d PDU A -1
H4 H 0.7572 0.4142 0.9674 0.136 Uiso 0.50 1 calc PR A -1
C5 C 0.816(3) 0.568(2) 0.8814(11) 0.109(5) Uani 0.50 1 d PDU A -1
H5 H 0.7856 0.5154 0.8329 0.130 Uiso 0.50 1 calc PR A -1
C6 C 0.884(3) 0.706(2) 0.8786(12) 0.079(4) Uani 0.50 1 d PDU A -1
H6 H 0.9060 0.7437 0.8250 0.094 Uiso 0.50 1 calc PR A -1
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'
Si Si 0.0817 0.0704 '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'
Cl Cl 0.1484 0.1585 '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
N2 Pd1 N2 171.1(7) 2_775 .
N2 Pd1 N2 89.65(6) 4_575 .
N2 Pd1 N2 89.65(6) . 3_755
N2 Pd1 Si1 85.5(4) 2_775 .
N2 Pd1 Si1 85.5(4) 4_575 .
N2 Pd1 Si1 85.5(4) . .
N2 Pd1 Si1 85.5(4) 3_755 .
N1 Si1 N1 171.5(8) 2_775 .
N1 Si1 N1 89.69(6) . 4_575
N1 Si1 N1 89.69(6) . 3_755
N1 Si1 Cl2 94.2(4) 2_775 .
N1 Si1 Cl2 94.2(4) . .
N1 Si1 Cl2 94.2(4) 4_575 .
N1 Si1 Cl2 94.2(4) 3_755 .
N1 Si1 Pd1 85.8(4) 2_775 .
N1 Si1 Pd1 85.8(4) . .
N1 Si1 Pd1 85.8(4) 4_575 .
N1 Si1 Pd1 85.8(4) 3_755 .
Cl2 Si1 Pd1 180.000(4) . .
C7 N1 C1 106.7(12) . .
C7 N1 Si1 123.6(9) . .
C1 N1 Si1 129.7(11) . .
C2 C1 N1 108.1(16) . .
C2 C1 H1 125.9 . .
N1 C1 H1 125.9 . .
C3 C2 C1 109.5(18) . .
C3 C2 H2 125.2 . .
C1 C2 H2 125.2 . .
C7 N2 C6 115.7(11) . .
C7 N2 Pd1 119.7(9) . .
C6 N2 Pd1 124.4(11) . .
N2 C7 N1 125.2(8) . .
N2 C7 C3 123.9(11) . .
N1 C7 C3 110.8(11) . .
C4 C3 C2 138.4(15) . .
C4 C3 C7 116.8(12) . .
C2 C3 C7 104.8(15) . .
C3 C4 C5 122.0(13) . .
C3 C4 H4 119.0 . .
C5 C4 H4 119.0 . .
C4 C5 C6 114.4(17) . .
C4 C5 H5 122.8 . .
C6 C5 H5 122.8 . .
N2 C6 C5 127.0(18) . .
N2 C6 H6 116.5 . .
C5 C6 H6 116.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd1 N2 2.012(12)
Pd1 Si1 2.641(10)
Si1 N1 1.902(14)
Si1 Cl2 2.04(2)
N1 C7 1.349(16)
N1 C1 1.413(14)
C1 C2 1.388(10)
C1 H1 0.9500
C2 C3 1.385(10)
C2 H2 0.9500
N2 C7 1.298(17)
N2 C6 1.337(16)
C7 C3 1.433(12)
C3 C4 1.351(19)
C4 C5 1.384(10)
C4 H4 0.9500
C5 C6 1.385(10)
C5 H5 0.9500
C6 H6 0.9500
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N2 Pd1 Si1 N1 -3.8(10) 2_775 2_775
N2 Pd1 Si1 N1 -93.8(10) 4_575 2_775
N2 Pd1 Si1 N1 176.2(10) . 2_775
N2 Pd1 Si1 N1 86.2(10) 3_755 2_775
N2 Pd1 Si1 N1 176.2(10) 2_775 .
N2 Pd1 Si1 N1 86.2(10) 4_575 .
N2 Pd1 Si1 N1 -3.8(10) . .
N2 Pd1 Si1 N1 -93.8(10) 3_755 .
N2 Pd1 Si1 N1 86.2(10) 2_775 4_575
N2 Pd1 Si1 N1 -3.8(10) 4_575 4_575
N2 Pd1 Si1 N1 -93.8(10) . 4_575
N2 Pd1 Si1 N1 176.2(10) 3_755 4_575
N2 Pd1 Si1 N1 -93.8(10) 2_775 3_755
N2 Pd1 Si1 N1 176.2(10) 4_575 3_755
N2 Pd1 Si1 N1 86.2(10) . 3_755
N2 Pd1 Si1 N1 -3.8(10) 3_755 3_755
N1 Si1 N1 C7 91.1(15) 4_575 .
N1 Si1 N1 C7 -80.4(16) 3_755 .
Cl2 Si1 N1 C7 -174.6(15) . .
Pd1 Si1 N1 C7 5.4(15) . .
N1 Si1 N1 C1 -92(2) 4_575 .
N1 Si1 N1 C1 96(2) 3_755 .
Cl2 Si1 N1 C1 2(2) . .
Pd1 Si1 N1 C1 -178(2) . .
C7 N1 C1 C2 -1(3) . .
Si1 N1 C1 C2 -178(2) . .
N1 C1 C2 C3 0(4) . .
N2 Pd1 N2 C7 -82.3(12) 4_575 .
N2 Pd1 N2 C7 88.8(13) 3_755 .
Si1 Pd1 N2 C7 3.2(12) . .
N2 Pd1 N2 C6 92(2) 4_575 .
N2 Pd1 N2 C6 -97(2) 3_755 .
Si1 Pd1 N2 C6 178(2) . .
C6 N2 C7 N1 -175(2) . .
Pd1 N2 C7 N1 -0.4(16) . .
C6 N2 C7 C3 0(2) . .
Pd1 N2 C7 C3 175.3(8) . .
C1 N1 C7 N2 178(2) . .
Si1 N1 C7 N2 -4.7(19) . .
C1 N1 C7 C3 2(2) . .
Si1 N1 C7 C3 179.2(10) . .
C1 C2 C3 C4 -177.7(19) . .
C1 C2 C3 C7 2(3) . .
N2 C7 C3 C4 1.0(18) . .
N1 C7 C3 C4 177.2(13) . .
N2 C7 C3 C2 -178(2) . .
N1 C7 C3 C2 -2(2) . .
C2 C3 C4 C5 175.0(18) . .
C7 C3 C4 C5 -4(2) . .
C3 C4 C5 C6 6(3) . .
C7 N2 C6 C5 1(4) . .
Pd1 N2 C6 C5 -173(2) . .
C4 C5 C6 N2 -4(4) . .
