#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:38:37 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180347 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/16/7201676.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_7201676
loop_
_publ_author_name
'Kalf, Irmgard'
'Wang, Ruimin'
'Englert, Ulli'
_publ_section_title
;
 A robust conglomerate structure type in salts of cationic
 organopalladium complexes and non-coordinating anions
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              39
_journal_paper_doi               10.1039/b712641g
_journal_volume                  10
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C15 H28 N3 Pd, B F4'
_chemical_formula_sum            'C15 H28 B F4 N3 Pd'
_chemical_formula_weight         443.61
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   10.824(3)
_cell_length_b                   12.230(3)
_cell_length_c                   14.106(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    278(2)
_cell_measurement_theta_max      16.0
_cell_measurement_theta_min      9.5
_cell_volume                     1867.3(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      278(2)
_diffrn_measured_fraction_theta_full .996
_diffrn_measured_fraction_theta_max .996
_diffrn_measurement_device_type  Enraf_Nonius_CAD4
_diffrn_measurement_method       θ/2θ
_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  0.0705
_diffrn_reflns_av_sigmaI/netI    0.0881
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13053
_diffrn_reflns_theta_full        28.03
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.033
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   empirical-psi
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         .661
_refine_diff_density_min         -.543
_refine_diff_density_rms         .098
_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   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4514
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0493
_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)+(0.0340P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0873
_reflns_number_gt                3308
_reflns_number_total             4514
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b712641g.txt
_cod_data_source_block           1b
_cod_database_code               7201676
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'
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 0.35568(4) 0.38131(3) 0.52812(3) 0.02869(10) Uani 1 1 d . . .
N1 N 0.2747(4) 0.3972(4) 0.6673(3) 0.0358(11) Uani 1 1 d . . .
N2 N 0.4079(4) 0.5444(4) 0.5487(3) 0.0386(12) Uani 1 1 d . . .
N3 N 0.2886(4) 0.2265(4) 0.5026(3) 0.0387(12) Uani 1 1 d . . .
H3A H 0.3472 0.1764 0.5152 0.046 Uiso 1 1 calc R . .
H3B H 0.2231 0.2131 0.5402 0.046 Uiso 1 1 calc R . .
C1 C 0.3189(6) 0.5018(5) 0.7061(4) 0.0481(18) Uani 1 1 d . . .
H1A H 0.3999 0.4922 0.7343 0.058 Uiso 1 1 calc R . .
H1B H 0.2628 0.5274 0.7549 0.058 Uiso 1 1 calc R . .
C2 C 0.3258(6) 0.5846(5) 0.6264(4) 0.0459(18) Uani 1 1 d . . .
H2A H 0.2436 0.5977 0.6015 0.055 Uiso 1 1 calc R . .
H2B H 0.3576 0.6533 0.6508 0.055 Uiso 1 1 calc R . .
C3 C 0.1376(6) 0.3973(5) 0.6577(4) 0.0508(15) Uani 1 1 d . . .
H3C H 0.1007 0.4127 0.7182 0.076 Uiso 1 1 calc R . .
H3D H 0.1104 0.3269 0.6360 0.076 Uiso 1 1 calc R . .
H3E H 0.1133 0.4522 0.6129 0.076 Uiso 1 1 calc R . .
C4 C 0.3101(6) 0.3072(5) 0.7327(4) 0.0493(18) Uani 1 1 d . . .
H4A H 0.3978 0.3089 0.7430 0.074 Uiso 1 1 calc R . .
H4B H 0.2874 0.2382 0.7052 0.074 Uiso 1 1 calc R . .
H4C H 0.2681 0.3163 0.7921 0.074 Uiso 1 1 calc R . .
C5 C 0.3811(6) 0.6157(5) 0.4659(5) 0.0639(19) Uani 1 1 d . . .
H5A H 0.3988 0.6903 0.4819 0.096 Uiso 1 1 calc R . .
H5B H 0.2956 0.6089 0.4489 0.096 Uiso 1 1 calc R . .
H5C H 0.4317 0.5938 0.4133 0.096 Uiso 1 1 calc R . .
C6 C 0.5383(6) 0.5575(6) 0.5761(5) 0.064(2) Uani 1 1 d . . .
H6A H 0.5901 0.5241 0.5291 0.096 Uiso 1 1 calc R . .
H6B H 0.5520 0.5230 0.6363 0.096 Uiso 1 1 calc R . .
H6C H 0.5576 0.6339 0.5808 0.096 Uiso 1 1 calc R . .
C7 C 0.2514(5) 0.2198(5) 0.4011(4) 0.0412(15) Uani 1 1 d . . .
H7 H 0.2480 0.1429 0.3818 0.049 Uiso 1 1 calc R . .
C8 C 0.3531(6) 0.2764(4) 0.3476(3) 0.0310(11) Uani 1 1 d . . .
C9 C 0.4197(5) 0.3578(4) 0.3955(3) 0.0318(13) Uani 1 1 d . . .
C10 C 0.5178(5) 0.4078(4) 0.3489(4) 0.0333(13) Uani 1 1 d . . .
H10 H 0.5670 0.4577 0.3812 0.040 Uiso 1 1 calc R . .
C11 C 0.5434(5) 0.3839(5) 0.2537(4) 0.0352(12) Uani 1 1 d . . .
C12 C 0.4717(6) 0.3094(5) 0.2071(4) 0.0380(14) Uani 1 1 d . . .
H12 H 0.4865 0.2956 0.1433 0.046 Uiso 1 1 calc R . .
C13 C 0.3769(5) 0.2537(5) 0.2529(4) 0.0387(14) Uani 1 1 d . . .
H13 H 0.3301 0.2019 0.2206 0.046 Uiso 1 1 calc R . .
C14 C 0.6473(7) 0.4455(5) 0.2040(4) 0.0512(16) Uani 1 1 d . . .
H14A H 0.6881 0.3976 0.1601 0.077 Uiso 1 1 calc R . .
H14B H 0.7057 0.4710 0.2502 0.077 Uiso 1 1 calc R . .
H14C H 0.6136 0.5069 0.1703 0.077 Uiso 1 1 calc R . .
C15 C 0.1278(6) 0.2708(6) 0.3869(4) 0.0589(18) Uani 1 1 d . . .
H15A H 0.1312 0.3464 0.4051 0.088 Uiso 1 1 calc R . .
H15B H 0.0678 0.2336 0.4252 0.088 Uiso 1 1 calc R . .
H15C H 0.1048 0.2654 0.3214 0.088 Uiso 1 1 calc R . .
F1 F -0.0015(9) 0.0969(9) 0.0524(5) 0.221(4) Uani 1 1 d . . .
F2 F 0.2024(7) 0.0822(9) 0.0567(5) 0.218(5) Uani 1 1 d . . .
F3 F 0.0921(6) 0.0925(10) 0.1788(5) 0.202(4) Uani 1 1 d . . .
F4 F 0.0846(9) -0.0377(6) 0.0927(11) 0.306(8) Uani 1 1 d . . .
B1 B 0.0959(9) 0.0578(9) 0.0940(7) 0.064(2) 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 .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B .0013 .0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -.9988 1.0072 '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
C9 Pd1 N3 80.1(2) . . ?
C9 Pd1 N2 99.9(2) . . ?
N3 Pd1 N2 174.5(2) . . ?
C9 Pd1 N1 175.2(2) . . ?
N3 Pd1 N1 95.63(17) . . ?
N2 Pd1 N1 84.14(17) . . ?
C1 N1 C4 109.2(4) . . ?
C1 N1 C3 110.9(5) . . ?
C4 N1 C3 108.3(5) . . ?
C1 N1 Pd1 106.5(3) . . ?
C4 N1 Pd1 113.1(3) . . ?
C3 N1 Pd1 108.8(3) . . ?
C6 N2 C5 109.2(5) . . ?
C6 N2 C2 110.0(5) . . ?
C5 N2 C2 105.5(4) . . ?
C6 N2 Pd1 113.5(4) . . ?
C5 N2 Pd1 113.4(4) . . ?
C2 N2 Pd1 104.8(3) . . ?
C7 N3 Pd1 108.3(3) . . ?
C7 N3 H3A 110.0 . . ?
Pd1 N3 H3A 110.0 . . ?
C7 N3 H3B 110.0 . . ?
Pd1 N3 H3B 110.0 . . ?
H3A N3 H3B 108.4 . . ?
N1 C1 C2 108.7(5) . . ?
N1 C1 H1A 109.9 . . ?
C2 C1 H1A 109.9 . . ?
N1 C1 H1B 109.9 . . ?
C2 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
N2 C2 C1 110.7(5) . . ?
N2 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
N2 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
N1 C3 H3C 109.5 . . ?
N1 C3 H3D 109.5 . . ?
H3C C3 H3D 109.5 . . ?
N1 C3 H3E 109.5 . . ?
H3C C3 H3E 109.5 . . ?
H3D C3 H3E 109.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 C7 C15 110.4(5) . . ?
N3 C7 C8 105.0(4) . . ?
C15 C7 C8 113.4(5) . . ?
N3 C7 H7 109.3 . . ?
C15 C7 H7 109.3 . . ?
C8 C7 H7 109.3 . . ?
C13 C8 C9 120.7(5) . . ?
C13 C8 C7 121.8(5) . . ?
C9 C8 C7 117.4(5) . . ?
C10 C9 C8 118.5(5) . . ?
C10 C9 Pd1 129.7(4) . . ?
C8 C9 Pd1 111.8(4) . . ?
C9 C10 C11 120.8(5) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 H10 119.6 . . ?
C12 C11 C10 119.2(5) . . ?
C12 C11 C14 121.9(5) . . ?
C10 C11 C14 118.9(5) . . ?
C11 C12 C13 121.5(5) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 H12 119.2 . . ?
C8 C13 C12 119.0(5) . . ?
C8 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C7 C15 H15A 109.5 . . ?
C7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
F4 B1 F3 110.1(12) . . ?
F4 B1 F1 105.9(12) . . ?
F3 B1 F1 106.1(9) . . ?
F4 B1 F2 108.3(10) . . ?
F3 B1 F2 109.4(10) . . ?
F1 B1 F2 116.9(9) . . ?
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
Pd1 C9 2.015(5) . ?
Pd1 N3 2.059(5) . ?
Pd1 N2 2.093(4) . ?
Pd1 N1 2.159(4) . ?
N1 C1 1.472(7) . ?
N1 C4 1.486(7) . ?
N1 C3 1.490(7) . ?
N2 C6 1.472(8) . ?
N2 C5 1.486(7) . ?
N2 C2 1.494(7) . ?
N3 C7 1.489(7) . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
C1 C2 1.515(8) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3C 0.9600 . ?
C3 H3D 0.9600 . ?
C3 H3E 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C15 1.490(9) . ?
C7 C8 1.504(8) . ?
C7 H7 0.9800 . ?
C8 C13 1.389(7) . ?
C8 C9 1.402(8) . ?
C9 C10 1.391(7) . ?
C10 C11 1.402(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.366(8) . ?
C11 C14 1.524(8) . ?
C12 C13 1.391(8) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
F1 B1 1.298(11) . ?
F2 B1 1.302(10) . ?
F3 B1 1.270(10) . ?
F4 B1 1.175(12) . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 Pd1 N1 C1 -158(2) . . . . ?
N3 Pd1 N1 C1 175.4(4) . . . . ?
N2 Pd1 N1 C1 -10.2(4) . . . . ?
C9 Pd1 N1 C4 82(2) . . . . ?
N3 Pd1 N1 C4 55.4(4) . . . . ?
N2 Pd1 N1 C4 -130.2(4) . . . . ?
C9 Pd1 N1 C3 -38(3) . . . . ?
N3 Pd1 N1 C3 -65.0(4) . . . . ?
N2 Pd1 N1 C3 109.4(4) . . . . ?
C9 Pd1 N2 C6 -81.1(4) . . . . ?
N3 Pd1 N2 C6 -170.7(18) . . . . ?
N1 Pd1 N2 C6 101.5(4) . . . . ?
C9 Pd1 N2 C5 44.3(4) . . . . ?
N3 Pd1 N2 C5 -45(2) . . . . ?
N1 Pd1 N2 C5 -133.1(4) . . . . ?
C9 Pd1 N2 C2 158.9(4) . . . . ?
N3 Pd1 N2 C2 69(2) . . . . ?
N1 Pd1 N2 C2 -18.5(4) . . . . ?
C9 Pd1 N3 C7 -36.4(4) . . . . ?
N2 Pd1 N3 C7 54(2) . . . . ?
N1 Pd1 N3 C7 141.4(4) . . . . ?
C4 N1 C1 C2 159.4(5) . . . . ?
C3 N1 C1 C2 -81.3(6) . . . . ?
Pd1 N1 C1 C2 36.9(5) . . . . ?
C6 N2 C2 C1 -77.2(6) . . . . ?
C5 N2 C2 C1 165.1(5) . . . . ?
Pd1 N2 C2 C1 45.2(5) . . . . ?
N1 C1 C2 N2 -57.2(6) . . . . ?
Pd1 N3 C7 C15 -80.0(5) . . . . ?
Pd1 N3 C7 C8 42.6(5) . . . . ?
N3 C7 C8 C13 155.8(5) . . . . ?
C15 C7 C8 C13 -83.5(7) . . . . ?
N3 C7 C8 C9 -27.4(7) . . . . ?
C15 C7 C8 C9 93.3(7) . . . . ?
C13 C8 C9 C10 -6.0(8) . . . . ?
C7 C8 C9 C10 177.1(5) . . . . ?
C13 C8 C9 Pd1 175.1(5) . . . . ?
C7 C8 C9 Pd1 -1.7(6) . . . . ?
N3 Pd1 C9 C10 -157.7(5) . . . . ?
N2 Pd1 C9 C10 27.9(5) . . . . ?
N1 Pd1 C9 C10 175(2) . . . . ?
N3 Pd1 C9 C8 21.0(4) . . . . ?
N2 Pd1 C9 C8 -153.4(4) . . . . ?
N1 Pd1 C9 C8 -6(3) . . . . ?
C8 C9 C10 C11 5.0(8) . . . . ?
Pd1 C9 C10 C11 -176.4(4) . . . . ?
C9 C10 C11 C12 -0.9(8) . . . . ?
C9 C10 C11 C14 176.6(5) . . . . ?
C10 C11 C12 C13 -2.5(8) . . . . ?
C14 C11 C12 C13 -179.9(6) . . . . ?
C9 C8 C13 C12 2.8(9) . . . . ?
C7 C8 C13 C12 179.5(5) . . . . ?
C11 C12 C13 C8 1.5(9) . . . . ?
