#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:53:40 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178922 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/51/4115195.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_4115195
loop_
_publ_author_name
'Myeongsoon Kang'
'Ayusman Sen'
'Lev Zakharov'
'Arnold L. Rheingold'
_publ_section_title
;
 Diametrically Opposite Trends in Alkene Insertion in Late and Early
 Transition Metal Compounds: Relevance to Transition-Metal-Catalyzed
 Polymerization of Polar Vinyl Monomers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12080
_journal_page_last               12081
_journal_paper_doi               10.1021/ja026550+
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C58 H84 Al2 Cl14 N4 Pd2'
_chemical_formula_weight         800.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                117.8510(10)
_cell_angle_beta                 117.3740(10)
_cell_angle_gamma                91.0630(10)
_cell_formula_units_Z            1
_cell_length_a                   12.9031(6)
_cell_length_b                   13.3823(7)
_cell_length_c                   13.8935(7)
_cell_measurement_temperature    100(2)
_cell_volume                     1798.51(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11565
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    1.082
_exptl_absorpt_correction_T_max  0.9479
_exptl_absorpt_correction_T_min  0.7372
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_meas      0
_exptl_crystal_description       blades
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         8060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0300P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0763
_reflns_number_gt                6652
_reflns_number_total             8060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0265502B_s2.cif
_cod_data_source_block           sen13
_cod_database_code               4115195
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Pd1 Pd 0.550332(16) 0.574824(16) 0.659293(17) 0.01301(6) Uani 1 1 d .
Al1 Al 0.28197(7) 1.32651(7) 0.67039(7) 0.01750(16) Uani 1 1 d .
Cl1 Cl 0.40999(5) 0.57663(5) 0.47997(5) 0.01847(13) Uani 1 1 d .
Cl2 Cl 0.31256(6) 1.17529(6) 0.68281(6) 0.02510(15) Uani 1 1 d .
Cl3 Cl 0.10060(6) 1.32616(6) 0.62806(7) 0.02589(15) Uani 1 1 d .
Cl4 Cl 0.40957(6) 1.48427(6) 0.85045(6) 0.02350(14) Uani 1 1 d .
Cl5 Cl 0.30474(6) 1.31631(6) 0.52439(6) 0.02634(15) Uani 1 1 d .
Cl6 Cl 1.03256(9) 0.89623(7) 1.35933(8) 0.0472(2) Uani 1 1 d .
Cl7 Cl 0.92194(8) 1.01678(8) 1.22618(8) 0.0463(2) Uani 1 1 d .
N1 N 0.51898(17) 0.70143(17) 0.78393(18) 0.0132(4) Uani 1 1 d .
N2 N 0.67058(18) 0.58147(17) 0.81899(18) 0.0141(4) Uani 1 1 d .
C1 C 0.5591(2) 0.8014(2) 1.0033(2) 0.0220(6) Uani 1 1 d .
H1A H 0.4975 0.8384 0.9724 0.033 Uiso 1 1 calc R
H1B H 0.6374 0.8626 1.0737 0.033 Uiso 1 1 calc R
H1C H 0.5331 0.7594 1.0340 0.033 Uiso 1 1 calc R
C2 C 0.5734(2) 0.7162(2) 0.8966(2) 0.0158(5) Uani 1 1 d .
C3 C 0.6619(2) 0.6476(2) 0.9170(2) 0.0153(5) Uani 1 1 d .
C4 C 0.7398(2) 0.6641(2) 1.0452(2) 0.0213(6) Uani 1 1 d .
H4A H 0.7920 0.6119 1.0406 0.032 Uiso 1 1 calc R
H4B H 0.6878 0.6446 1.0715 0.032 Uiso 1 1 calc R
H4C H 0.7911 0.7466 1.1080 0.032 Uiso 1 1 calc R
C5 C 0.7677(2) 0.5272(2) 0.8256(2) 0.0169(5) Uani 1 1 d .
C6 C 0.7473(2) 0.4074(2) 0.7863(2) 0.0198(5) Uani 1 1 d .
C7 C 0.8401(2) 0.3583(2) 0.7823(3) 0.0259(6) Uani 1 1 d .
H7A H 0.8293 0.2776 0.7570 0.031 Uiso 1 1 calc R
C8 C 0.9471(2) 0.4229(3) 0.8141(3) 0.0274(6) Uani 1 1 d .
H8A H 1.0084 0.3865 0.8090 0.033 Uiso 1 1 calc R
C9 C 0.9655(3) 0.5411(3) 0.8535(3) 0.0269(6) Uani 1 1 d .
H9A H 1.0401 0.5854 0.8761 0.032 Uiso 1 1 calc R
C10 C 0.8771(2) 0.5958(2) 0.8605(2) 0.0203(5) Uani 1 1 d .
C11 C 0.8999(2) 0.7261(2) 0.9014(3) 0.0245(6) Uani 1 1 d .
H11A H 0.8337 0.7537 0.9153 0.029 Uiso 1 1 calc R
C12 C 0.8922(4) 0.7386(3) 0.7959(3) 0.0507(10) Uani 1 1 d .
H12A H 0.8127 0.6887 0.7167 0.076 Uiso 1 1 calc R
H12B H 0.9575 0.7137 0.7817 0.076 Uiso 1 1 calc R
H12C H 0.9016 0.8214 0.8210 0.076 Uiso 1 1 calc R
C13 C 1.0221(3) 0.8046(3) 1.0269(3) 0.0404(8) Uani 1 1 d .
H13A H 1.0328 0.8869 1.0497 0.061 Uiso 1 1 calc R
H13B H 1.0887 0.7784 1.0163 0.061 Uiso 1 1 calc R
H13C H 1.0235 0.7989 1.0952 0.061 Uiso 1 1 calc R
C14 C 0.6308(2) 0.3341(2) 0.7526(3) 0.0233(6) Uani 1 1 d .
H14A H 0.5681 0.3771 0.7391 0.028 Uiso 1 1 calc R
C15 C 0.6553(3) 0.3211(3) 0.8644(3) 0.0330(7) Uani 1 1 d .
H15A H 0.6873 0.3997 0.9425 0.049 Uiso 1 1 calc R
H15B H 0.7153 0.2775 0.8778 0.049 Uiso 1 1 calc R
H15C H 0.5789 0.2777 0.8444 0.049 Uiso 1 1 calc R
C16 C 0.5795(3) 0.2116(2) 0.6290(3) 0.0312(7) Uani 1 1 d .
H16A H 0.5640 0.2211 0.5581 0.047 Uiso 1 1 calc R
H16B H 0.5030 0.1684 0.6087 0.047 Uiso 1 1 calc R
H16C H 0.6389 0.1672 0.6411 0.047 Uiso 1 1 calc R
C17 C 0.4449(2) 0.7737(2) 0.7504(2) 0.0154(5) Uani 1 1 d .
C18 C 0.3181(2) 0.7337(2) 0.6880(2) 0.0177(5) Uani 1 1 d .
C19 C 0.2515(2) 0.8025(2) 0.6502(3) 0.0247(6) Uani 1 1 d .
H19A H 0.1650 0.7779 0.6085 0.030 Uiso 1 1 calc R
C20 C 0.3077(2) 0.9054(2) 0.6715(3) 0.0257(6) Uani 1 1 d .
H20A H 0.2603 0.9509 0.6445 0.031 Uiso 1 1 calc R
C21 C 0.4339(2) 0.9425(2) 0.7326(3) 0.0237(6) Uani 1 1 d .
H21A H 0.4720 1.0136 0.7471 0.028 Uiso 1 1 calc R
C22 C 0.5059(2) 0.8780(2) 0.7733(2) 0.0192(5) Uani 1 1 d .
C23 C 0.2515(2) 0.6205(2) 0.6615(2) 0.0200(5) Uani 1 1 d .
H23A H 0.3120 0.5771 0.6830 0.024 Uiso 1 1 calc R
C24 C 0.1502(2) 0.5397(2) 0.5197(3) 0.0243(6) Uani 1 1 d .
H24A H 0.1854 0.5215 0.4664 0.036 Uiso 1 1 calc R
H24B H 0.0888 0.5799 0.4971 0.036 Uiso 1 1 calc R
H24C H 0.1117 0.4661 0.5051 0.036 Uiso 1 1 calc R
C25 C 0.1993(3) 0.6501(2) 0.7481(3) 0.0287(6) Uani 1 1 d .
H25A H 0.2655 0.7012 0.8383 0.043 Uiso 1 1 calc R
H25B H 0.1607 0.5768 0.7340 0.043 Uiso 1 1 calc R
H25C H 0.1383 0.6912 0.7273 0.043 Uiso 1 1 calc R
C26 C 0.6440(2) 0.9202(2) 0.8369(3) 0.0261(6) Uani 1 1 d .
H26A H 0.6792 0.8603 0.8544 0.031 Uiso 1 1 calc R
C27 C 0.7006(3) 1.0390(3) 0.9651(3) 0.0351(7) Uani 1 1 d .
H27A H 0.6796 1.0312 1.0212 0.053 Uiso 1 1 calc R
H27B H 0.6687 1.0994 0.9498 0.053 Uiso 1 1 calc R
H27C H 0.7897 1.0625 1.0064 0.053 Uiso 1 1 calc R
C28 C 0.6760(3) 0.9298(3) 0.7475(3) 0.0420(8) Uani 1 1 d .
H28A H 0.6395 0.8531 0.6663 0.063 Uiso 1 1 calc R
H28B H 0.7650 0.9530 0.7883 0.063 Uiso 1 1 calc R
H28C H 0.6439 0.9895 0.7308 0.063 Uiso 1 1 calc R
C29 C 1.0449(3) 1.0296(3) 1.3641(3) 0.0406(8) Uani 1 1 d .
H29A H 1.1225 1.0536 1.3713 0.049 Uiso 1 1 calc R
H29B H 1.0474 1.0924 1.4411 0.049 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'
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'
Al Al 0.0645 0.0514 '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'
Pd Pd -0.9988 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_3
N1 Pd1 N2 80.35(8) .
N1 Pd1 Cl1 96.87(6) .
N2 Pd1 Cl1 177.06(6) .
N1 Pd1 Cl1 177.26(6) 2_666
N2 Pd1 Cl1 97.21(6) 2_666
Cl1 Pd1 Cl1 85.60(2) 2_666
Cl5 Al1 Cl3 111.29(4) .
Cl5 Al1 Cl2 109.39(4) .
Cl3 Al1 Cl2 107.42(4) .
Cl5 Al1 Cl4 109.66(4) .
Cl3 Al1 Cl4 109.45(4) .
Cl2 Al1 Cl4 109.59(4) .
Pd1 Cl1 Pd1 94.40(2) 2_666
C2 N1 C17 123.7(2) .
C2 N1 Pd1 114.65(16) .
C17 N1 Pd1 121.61(15) .
C3 N2 C5 123.6(2) .
C3 N2 Pd1 114.54(16) .
C5 N2 Pd1 121.42(15) .
N1 C2 C3 114.6(2) .
N1 C2 C1 124.3(2) .
C3 C2 C1 120.8(2) .
N2 C3 C4 124.2(2) .
N2 C3 C2 114.9(2) .
C4 C3 C2 120.8(2) .
C6 C5 C10 122.2(2) .
C6 C5 N2 120.3(2) .
C10 C5 N2 117.2(2) .
C7 C6 C5 117.0(2) .
C7 C6 C14 120.7(2) .
C5 C6 C14 122.3(2) .
C8 C7 C6 121.9(3) .
C7 C8 C9 120.0(3) .
C8 C9 C10 121.1(3) .
C9 C10 C5 117.8(2) .
C9 C10 C11 119.4(2) .
C5 C10 C11 122.8(2) .
C12 C11 C13 110.7(3) .
C12 C11 C10 110.3(2) .
C13 C11 C10 112.2(2) .
C6 C14 C15 109.7(2) .
C6 C14 C16 112.0(2) .
C15 C14 C16 110.2(2) .
C18 C17 C22 122.8(2) .
C18 C17 N1 120.0(2) .
C22 C17 N1 117.0(2) .
C19 C18 C17 117.4(2) .
C19 C18 C23 119.5(2) .
C17 C18 C23 123.1(2) .
C20 C19 C18 121.6(3) .
C19 C20 C21 119.7(3) .
C20 C21 C22 121.6(2) .
C21 C22 C17 116.9(2) .
C21 C22 C26 119.9(2) .
C17 C22 C26 123.2(2) .
C18 C23 C24 111.5(2) .
C18 C23 C25 110.1(2) .
C24 C23 C25 110.8(2) .
C22 C26 C28 110.7(2) .
C22 C26 C27 110.8(2) .
C28 C26 C27 110.6(2) .
Cl6 C29 Cl7 111.97(17) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N1 1.990(2) .
Pd1 N2 1.9958(19) .
Pd1 Cl1 2.3230(6) .
Pd1 Cl1 2.3236(6) 2_666
Al1 Cl5 2.1238(10) .
Al1 Cl3 2.1340(10) .
Al1 Cl2 2.1388(10) .
Al1 Cl4 2.1389(10) .
Cl1 Pd1 2.3236(6) 2_666
Cl6 C29 1.757(3) .
Cl7 C29 1.762(3) .
N1 C2 1.295(3) .
N1 C17 1.453(3) .
N2 C3 1.292(3) .
N2 C5 1.448(3) .
C1 C2 1.486(3) .
C2 C3 1.488(3) .
C3 C4 1.486(3) .
C5 C6 1.405(3) .
C5 C10 1.406(3) .
C6 C7 1.387(4) .
C6 C14 1.520(4) .
C7 C8 1.375(4) .
C8 C9 1.383(4) .
C9 C10 1.384(4) .
C10 C11 1.533(4) .
C11 C12 1.510(4) .
C11 C13 1.526(4) .
C14 C15 1.531(4) .
C14 C16 1.536(4) .
C17 C18 1.395(3) .
C17 C22 1.409(3) .
C18 C19 1.389(3) .
C18 C23 1.519(3) .
C19 C20 1.377(4) .
C20 C21 1.387(4) .
C21 C22 1.389(4) .
C22 C26 1.524(4) .
C23 C24 1.532(4) .
C23 C25 1.540(4) .
C26 C28 1.532(4) .
C26 C27 1.533(4) .
