#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/16/4111612.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_4111612
loop_
_publ_author_name
'B. Scott Williams'
'Mark D. Leatherman'
'Peter S. White'
'Maurice Brookhart'
_publ_section_title
;
 Reactions of Vinyl Acetate and Vinyl Trifluoroacetate with Cationic
 Diimine Pd(II) and Ni(II) Alkyl Complexes: Identification of Problems
 Connected with Copolymerizations of These Monomers with Ethylene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5132
_journal_page_last               5146
_journal_paper_doi               10.1021/ja045969s
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C33 H33 N2 O2 Pd, F6 Sb, 2(C H2 Cl2) '
_chemical_formula_sum            'C35 H37 Cl4 F6 N2 O2 Pd Sb'
_chemical_formula_weight         1001.63
_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'
_cell_angle_alpha                91.953(1)
_cell_angle_beta                 90.798(2)
_cell_angle_gamma                108.682(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8149(9)
_cell_length_b                   12.7183(13)
_cell_length_c                   18.3693(19)
_cell_measurement_reflns_used    4274
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.50
_cell_volume                     1949.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT/NRCVAX DATRD2'
_computing_molecular_graphics    NRCVAX
_computing_publication_material  'NRCVAX TABLES Jan 94 Version'
_computing_structure_refinement  'NRCVAX LSTSQ'
_computing_structure_solution    'NRCVAX SOLVER'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measurement_device       'Bruker SMART 1K'
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'xray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18479
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    1.49
_exptl_absorpt_correction_T_max  0.740
_exptl_absorpt_correction_T_min  0.597
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_description       block
_exptl_crystal_F_000             990.60
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.92
_refine_diff_density_min         -1.55
_refine_ls_extinction_coef       0.622(8)
_refine_ls_extinction_method     Larson
_refine_ls_goodness_of_fit_ref   2.56
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         5435
_refine_ls_R_factor_all          0.073
_refine_ls_R_factor_gt           0.057
_refine_ls_shift/su_max          0.008
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     1/(σ²(F)+0.0003F²)
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.084
_refine_ls_wR_factor_gt          0.076
_reflns_number_gt                5499
_reflns_number_total             6826
_reflns_threshold_expression     'Inet > 3.0σ(Inet)'
_cod_data_source_file            ja045969ssi20040706_052904.cif
_cod_data_source_block           c02055
_cod_original_formula_sum        'C35 H37 Cl4 F6 N2 O2 Pd Sb  '
_cod_database_code               4111612
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_refinement_flags
_atom_site_type_symbol
Pd1 0.68425(7) 0.27365(4) 0.29476(3) 0.0293(3) Uani . Pd
N1 0.5011(7) 0.1251(5) 0.2803(3) 0.028(3) Uani . n
C2 0.4034(9) 0.1258(6) 0.2284(4) 0.027(4) Uani . C
C3 0.2470(9) 0.0469(6) 0.2016(4) 0.027(4) Uani . C
C4 0.1924(9) 0.1030(6) 0.1470(4) 0.027(4) Uani . C
C5 0.2964(8) 0.2116(5) 0.1361(4) 0.024(4) Uani . C
C6 0.4315(9) 0.2290(6) 0.1859(4) 0.027(4) Uani . C
N7 0.5596(7) 0.3112(5) 0.2030(3) 0.030(3) Uani . n
C8 0.1561(10) -0.0575(6) 0.2195(4) 0.035(5) Uani . C
C9 0.0088(10) -0.1073(7) 0.1809(5) 0.042(5) Uani . C
C10 -0.0454(10) -0.0518(7) 0.1275(4) 0.040(4) Uani . C
C11 0.0442(9) 0.0574(6) 0.1088(4) 0.030(4) Uani . C
C12 0.0065(9) 0.1244(7) 0.0587(4) 0.037(5) Uani . C
C13 0.1068(10) 0.2308(6) 0.0468(4) 0.037(5) Uani . C
C14 0.2557(9) 0.2769(6) 0.0855(4) 0.030(4) Uani . C
C15 0.4665(9) 0.0301(6) 0.3256(4) 0.031(4) Uani . C
C16 0.5135(10) -0.0606(6) 0.3032(4) 0.037(5) Uani . C
C17 0.4796(11) -0.1513(7) 0.3478(5) 0.046(5) Uani . C
C18 0.4038(11) -0.1485(7) 0.4130(5) 0.046(5) Uani . C
C19 0.3603(11) -0.0586(7) 0.4347(5) 0.047(5) Uani . C
C20 0.3932(10) 0.0353(6) 0.3909(4) 0.034(4) Uani . C
C21 0.5964(12) -0.0636(7) 0.2322(5) 0.052(6) Uani . C
C22 0.3488(11) 0.1345(7) 0.4152(5) 0.046(5) Uani . C
C23 0.5913(9) 0.4148(6) 0.1661(4) 0.033(4) Uani . C
C24 0.5424(11) 0.4984(7) 0.2019(4) 0.041(5) Uani . C
C25 0.5747(12) 0.5961(7) 0.1664(5) 0.046(6) Uani . C
C26 0.6453(12) 0.6129(7) 0.0995(5) 0.047(6) Uani . C
C27 0.6916(11) 0.5308(7) 0.0663(5) 0.047(5) Uani . C
C28 0.6639(10) 0.4279(6) 0.0993(4) 0.037(5) Uani . C
C29 0.4616(13) 0.4811(7) 0.2727(5) 0.058(7) Uani . C
C30 0.7080(12) 0.3353(7) 0.0600(6) 0.058(6) Uani . C
O31 0.8601(7) 0.4222(4) 0.3120(3) 0.041(3) Uani . O
C32 0.9343(10) 0.4255(7) 0.3716(5) 0.040(5) Uani . C
O33 0.9093(7) 0.3407(5) 0.4111(3) 0.048(4) Uani . O
C34 0.7916(9) 0.2363(6) 0.3823(4) 0.034(4) Uani . C
C35 1.0679(14) 0.5297(8) 0.3978(6) 0.068(7) Uani . C
C36 0.8831(12) 0.1555(8) 0.3665(5) 0.054(6) Uani . C
C37 1.0040(14) 0.1892(10) 0.3050(6) 0.079(8) Uani . C
Sb1 0.50000 0.50000 0.50000 0.0315(4) Uani S Sb
F11 0.4894(7) 0.6119(4) 0.4395(3) 0.054(3) Uani . F
F12 0.3407(7) 0.3959(4) 0.4423(3) 0.061(3) Uani . F
F13 0.6587(7) 0.4735(5) 0.4434(3) 0.062(4) Uani . F
Sb2 0.50000 1.00000 0.00000 0.0273(4) Uani S Sb
F21 0.5620(6) 1.0768(4) 0.09018(23) 0.043(3) Uani . F
F22 0.6211(6) 0.9072(4) 0.0217(3) 0.046(3) Uani . F
F23 0.3233(5) 0.9014(4) 0.04320(24) 0.043(3) Uani . F
C91 0.100(3) 0.6290(23) 0.1546(11) 0.33(4) Uani . C
Cl1 0.2118(5) 0.6811(3) 0.22333(25) 0.118(3) Uani . Cl
Cl2 0.0907(5) 0.4687(4) 0.1423(3) 0.157(4) Uani . Cl
C92 0.869(3) 0.7626(11) 0.4152(8) 0.148(18) Uani . C
Cl3 0.8285(5) 0.70302(24) 0.32625(16) 0.0872(24) Uani . Cl
Cl4 0.9334(4) 0.9063(3) 0.41428(21) 0.0983(24) Uani . Cl
H8 0.190 -0.096 0.257 0.0439 Uiso . H
H9 -0.055 -0.181 0.192 0.0497 Uiso . H
H10 -0.147 -0.088 0.103 0.0456 Uiso . H
H12 -0.092 0.096 0.031 0.0463 Uiso . H
H13 0.075 0.275 0.012 0.0466 Uiso . H
H14 0.325 0.350 0.077 0.0407 Uiso . H
H17 0.511 -0.214 0.333 0.0585 Uiso . H
H18 0.377 -0.212 0.443 0.0569 Uiso . H
H19 0.310 -0.057 0.480 0.0584 Uiso . H
H21a 0.618 -0.133 0.226 0.0662 Uiso . H
H21b 0.529 -0.056 0.193 0.0662 Uiso . H
H21c 0.695 -0.003 0.233 0.0662 Uiso . H
H22a 0.380 0.189 0.379 0.0569 Uiso . H
H22b 0.235 0.113 0.421 0.0569 Uiso . H
H22c 0.402 0.165 0.461 0.0569 Uiso . H
H25 0.542 0.655 0.189 0.0576 Uiso . H
H26 0.664 0.682 0.076 0.0567 Uiso . H
H27 0.744 0.543 0.020 0.0572 Uiso . H
H29a 0.440 0.547 0.289 0.0715 Uiso . H
H29b 0.362 0.421 0.266 0.0715 Uiso . H
H29c 0.528 0.462 0.308 0.0715 Uiso . H
H30a 0.757 0.361 0.015 0.0685 Uiso . H
H30b 0.782 0.314 0.090 0.0685 Uiso . H
H30c 0.613 0.273 0.051 0.0685 Uiso . H
H34 0.708 0.207 0.416 0.0425 Uiso . H
H35a 1.111 0.517 0.444 0.0748 Uiso . H
H35b 1.151 0.548 0.363 0.0748 Uiso . H
H35c 1.025 0.590 0.404 0.0748 Uiso . H
H36a 0.941 0.150 0.410 0.0643 Uiso . H
H36b 0.807 0.084 0.354 0.0643 Uiso . H
H37a 1.057 0.134 0.298 0.0948 Uiso . H
H37b 0.948 0.194 0.261 0.0948 Uiso . H
H37c 1.082 0.260 0.317 0.0948 Uiso . H
H91a 0.083 0.666 0.113 0.3919 Uiso . H
H91b 0.003 0.608 0.184 0.3862 Uiso . H
H92a 0.955 0.741 0.436 0.1545 Uiso . H
H92b 0.777 0.736 0.445 0.1546 Uiso . H
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pd -0.999 1.007 'International Tables Vol. IV Table 2.2B'
Sb -0.587 1.546 'International Tables Vol. IV Table 2.2B'
Cl 0.148 0.159 'International Tables Vol. IV Table 2.2B'
C 0.003 0.002 'International Tables Vol. IV Table 2.2B'
H 0.000 0.000 'International Tables Vol. IV Table 2.2B'
F 0.017 0.010 'International Tables Vol. IV Table 2.2B'
N 0.006 0.003 'International Tables Vol. IV Table 2.2B'
O 0.011 0.006 'International Tables Vol. IV Table 2.2B'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N(1) Pd(1) N(7) 80.19(22)
N(1) Pd(1) O(31) 177.79(23)
N(1) Pd(1) C(34) 98.2(3)
N(7) Pd(1) O(31) 100.05(22)
N(7) Pd(1) C(34) 177.6(3)
O(31) Pd(1) C(34) 81.4(3)
Pd(1) N(1) C(2) 112.9(5)
Pd(1) N(1) C(15) 127.4(5)
C(2) N(1) C(15) 119.5(6)
N(1) C(2) C(3) 133.9(7)
N(1) C(2) C(6) 119.3(6)
C(3) C(2) C(6) 106.4(6)
C(2) C(3) C(4) 105.4(6)
C(2) C(3) C(8) 134.4(7)
C(4) C(3) C(8) 120.3(7)
C(3) C(4) C(5) 113.9(6)
C(3) C(4) C(11) 123.5(6)
C(5) C(4) C(11) 122.6(7)
C(4) C(5) C(6) 106.3(6)
C(4) C(5) C(14) 120.0(6)
C(6) C(5) C(14) 133.7(6)
C(2) C(6) C(5) 108.0(6)
C(2) C(6) N(7) 116.6(6)
C(5) C(6) N(7) 135.3(6)
Pd(1) N(7) C(6) 110.9(5)
Pd(1) N(7) C(23) 129.2(4)
C(6) N(7) C(23) 119.6(6)
C(3) C(8) C(9) 118.0(7)
C(8) C(9) C(10) 121.7(7)
C(9) C(10) C(11) 121.8(7)
C(4) C(11) C(10) 114.8(7)
C(4) C(11) C(12) 116.2(7)
C(10) C(11) C(12) 129.0(7)
C(11) C(12) C(13) 122.3(7)
C(12) C(13) C(14) 121.5(7)
C(5) C(14) C(13) 117.4(7)
N(1) C(15) C(16) 119.1(7)
N(1) C(15) C(20) 117.8(6)
C(16) C(15) C(20) 123.0(7)
C(15) C(16) C(17) 118.2(7)
C(15) C(16) C(21) 122.1(7)
C(17) C(16) C(21) 119.7(7)
C(16) C(17) C(18) 119.8(7)
C(17) C(18) C(19) 121.3(8)
C(18) C(19) C(20) 120.6(8)
C(15) C(20) C(19) 117.1(7)
C(15) C(20) C(22) 122.3(7)
C(19) C(20) C(22) 120.7(7)
N(7) C(23) C(24) 116.4(7)
N(7) C(23) C(28) 120.4(6)
C(24) C(23) C(28) 123.2(7)
C(23) C(24) C(25) 115.4(8)
C(23) C(24) C(29) 122.0(7)
C(25) C(24) C(29) 122.5(7)
C(24) C(25) C(26) 123.5(7)
C(25) C(26) C(27) 119.7(8)
C(26) C(27) C(28) 120.4(8)
C(23) C(28) C(27) 117.6(7)
C(23) C(28) C(30) 122.5(7)
C(27) C(28) C(30) 119.8(7)
Pd(1) O(31) C(32) 111.2(5)
O(31) C(32) O(33) 122.6(7)
O(31) C(32) C(35) 120.9(8)
O(33) C(32) C(35) 116.4(7)
C(32) O(33) C(34) 116.7(6)
Pd(1) C(34) O(33) 107.0(4)
Pd(1) C(34) C(36) 114.4(6)
O(33) C(34) C(36) 106.9(6)
C(34) C(36) C(37) 114.5(8)
F(11) Sb(1) F(12) 89.93(23)
F(11) Sb(1) F(13) 90.77(23)
F(12) Sb(1) F(13) 90.5(3)
F(21) Sb(2) F(22) 90.15(20)
F(21) Sb(2) F(23) 89.69(20)
F(22) Sb(2) F(23) 89.69(21)
Cl(1) C(91) Cl(2) 107.5(10)
Cl(3) C(92) Cl(4) 111.1(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd(1) N(1) 2.061(6)
Pd(1) N(7) 2.148(6)
Pd(1) O(31) 2.035(5)
Pd(1) C(34) 2.001(7)
N(1) C(2) 1.278(9)
N(1) C(15) 1.443(9)
C(2) C(3) 1.487(10)
C(2) C(6) 1.504(10)
C(3) C(4) 1.415(10)
C(3) C(8) 1.366(10)
C(4) C(5) 1.415(10)
C(4) C(11) 1.413(10)
C(5) C(6) 1.445(10)
C(5) C(14) 1.386(10)
C(6) N(7) 1.296(9)
N(7) C(23) 1.450(9)
C(8) C(9) 1.416(12)
C(9) C(10) 1.392(13)
C(10) C(11) 1.417(11)
C(11) C(12) 1.381(11)
C(12) C(13) 1.386(11)
C(13) C(14) 1.422(11)
C(15) C(16) 1.396(10)
C(15) C(20) 1.380(11)
C(16) C(17) 1.394(11)
C(16) C(21) 1.508(12)
C(17) C(18) 1.385(13)
C(18) C(19) 1.366(13)
C(19) C(20) 1.418(11)
C(20) C(22) 1.491(11)
C(23) C(24) 1.415(11)
C(23) C(28) 1.382(11)
C(24) C(25) 1.373(11)
C(24) C(29) 1.480(13)
C(25) C(26) 1.377(13)
C(26) C(27) 1.365(12)
C(27) C(28) 1.412(11)
C(28) C(30) 1.518(12)
O(31) C(32) 1.260(10)
C(32) O(33) 1.281(11)
C(32) C(35) 1.522(13)
O(33) C(34) 1.474(9)
C(34) C(36) 1.519(12)
C(36) C(37) 1.539(15)
Sb(1) F(11) 1.860(4)
Sb(1) F(12) 1.877(5)
Sb(1) F(13) 1.863(5)
Sb(2) F(21) 1.876(4)
Sb(2) F(22) 1.875(4)
Sb(2) F(23) 1.865(4)
C(91) Cl(1) 1.579(14)
C(91) Cl(2) 2.018(22)
C(92) Cl(3) 1.761(14)
C(92) Cl(4) 1.733(14)
