#------------------------------------------------------------------------------
#$Date: 2016-01-27 04:20:33 +0200 (Wed, 27 Jan 2016) $
#$Revision: 175111 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/32/2003202.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_2003202
loop_
_publ_author_name
'Cross, Ronald J.'
'Kennedy, Alan R.'
'Muir, Kenneth W.'
_publ_section_title
;
 trans-Bromo(o-tolyl)bis(triphenylphosphine)palladium(II)
 from Crystals With and Without Stacking Faults
;
_journal_coeditor_code           HA1125
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              208
_journal_page_last               210
_journal_paper_doi               10.1107/S0108270194009042
_journal_volume                  51
_journal_year                    1995
_chemical_formula_sum            'C43 H37 Br P2 Pd'
_chemical_formula_weight         802.04
_chemical_melting_point          478
_chemical_name_systematic
;
 trans-bromo-ortho-tolyl-bis(triphenylphosphine)palladium(II)
;
_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     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                95.161(6)
_cell_angle_beta                 92.072(4)
_cell_angle_gamma                105.199(6)
_cell_formula_units_Z            2
_cell_length_a                   11.0691(4)
_cell_length_b                   12.1779(11)
_cell_length_c                   14.3380(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    299
_cell_measurement_theta_max      22.9
_cell_measurement_theta_min      20.8
_cell_volume                     1854.0(2)
_computing_cell_refinement       CAD4
_computing_data_collection       'CAD4 (Enraf-Nonius, 1992)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'CAMERON (Pierce & Watkin, 1994)'
_computing_publication_material  GX
_computing_structure_refinement  GX
_computing_structure_solution    'GX (Mallinson & Muir, 1985)'
_diffrn_ambient_temperature      299
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  C
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_number            19684
_diffrn_reflns_theta_max         24.6
_diffrn_reflns_theta_min         2.1
_diffrn_standards_decay_%        -0.9
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.68
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       needle
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.94
_refine_diff_density_min         -1.23
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   3.6
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         4392
_refine_ls_R_factor_obs          .060
_refine_ls_shift/esd_max         0.02
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(F) + 0.00023F²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         .095
_reflns_number_observed          4392
_reflns_number_total             18706
_reflns_observed_criterion       I>3.0\s(I)
_cod_database_code               2003202
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_thermal_displace_type
Pd(1) Pd -0.18548(7) 0.04221(6) 0.22481(6) 0.034 Uani
Br(1) Br 0.04060(12) 0.06261(12) 0.18901(12) 0.081 Uani
P(1) P -0.2179(2) -0.1476(2) 0.2531(2) 0.037 Uani
P(2) P -0.1598(2) 0.2345(2) 0.2068(2) 0.035 Uani
C(1) C -0.3713(9) 0.0199(8) 0.2323(8) 0.042 Uani
C(2) C -0.4310(10) 0.0376(8) 0.3117(9) 0.050 Uani
C(3) C -0.5625(12) 0.0240(11) 0.3077(11) 0.070 Uani
C(4) C -0.6265(14) -0.0134(14) 0.2227(16) 0.096 Uani
C(5) C -0.5736(16) -0.0365(14) 0.1438(15) 0.104 Uani
C(6) C -0.4416(11) -0.0179(10) 0.1452(10) 0.065 Uani
C(7) C -0.3595(12) 0.0756(11) 0.4003(9) 0.070 Uani
C(11) C -0.0822(9) -0.1788(9) 0.3120(7) 0.042 Uani
C(12) C -0.0007(12) -0.0952(10) 0.3716(8) 0.062 Uani
C(13) C 0.0966(13) -0.1197(13) 0.4209(10) 0.078 Uani
C(14) C 0.1160(12) -0.2221(14) 0.4100(9) 0.073 Uani
C(15) C 0.0373(13) -0.3100(13) 0.3494(9) 0.080 Uani
C(16) C -0.0642(11) -0.2885(10) 0.3001(8) 0.062 Uani
C(21) C -0.3456(9) -0.2095(8) 0.3271(7) 0.039 Uani
C(22) C -0.3145(11) -0.2210(10) 0.4216(8) 0.064 Uani
C(23) C -0.4145(17) -0.2604(11) 0.4790(9) 0.083 Uani
C(24) C -0.5371(15) -0.2898(11) 0.4442(11) 0.076 Uani
C(25) C -0.5648(12) -0.2786(10) 0.3540(11) 0.070 Uani
C(26) C -0.4685(10) -0.2352(10) 0.2960(8) 0.057 Uani
C(31) C -0.2540(9) -0.2396(9) 0.1443(7) 0.041 Uani
C(32) C -0.3226(10) -0.3574(9) 0.1388(8) 0.048 Uani
C(33) C -0.3499(11) -0.4232(9) 0.0546(9) 0.056 Uani
C(34) C -0.3140(12) -0.3763(12) -0.0276(9) 0.068 Uani
C(35) C -0.2457(12) -0.2659(11) -0.0241(8) 0.062 Uani
C(36) C -0.2177(10) -0.1968(8) 0.0604(8) 0.046 Uani
C(41) C -0.0123(9) 0.3171(8) 0.2691(7) 0.041 Uani
C(42) C 0.0829(10) 0.3908(9) 0.2281(8) 0.051 Uani
C(43) C 0.1910(11) 0.4457(11) 0.2778(10) 0.065 Uani
C(44) C 0.2092(10) 0.4323(12) 0.3726(10) 0.066 Uani
C(45) C 0.1156(11) 0.3604(12) 0.4141(9) 0.067 Uani
C(46) C 0.0083(11) 0.3013(10) 0.3608(8) 0.057 Uani
C(51) C -0.2748(9) 0.3083(8) 0.2499(7) 0.038 Uani
C(52) C -0.2432(11) 0.4013(9) 0.3209(8) 0.055 Uani
C(53) C -0.3293(12) 0.4562(10) 0.3486(8) 0.060 Uani
C(54) C -0.4471(14) 0.4212(12) 0.3106(10) 0.076 Uani
C(55) C -0.4818(11) 0.3332(11) 0.2418(10) 0.066 Uani
C(56) C -0.3966(11) 0.2779(10) 0.2132(9) 0.060 Uani
C(61) C -0.1446(9) 0.2707(9) 0.0875(7) 0.042 Uani
C(62) C -0.1597(13) 0.3727(11) 0.0606(8) 0.074 Uani
C(63) C -0.1519(16) 0.3944(12) -0.0323(9) 0.101 Uani
C(64) C -0.1234(14) 0.3183(15) -0.0990(9) 0.091 Uani
C(65) C -0.1048(12) 0.2182(11) -0.0742(8) 0.063 Uani
C(66) C -0.1170(10) 0.1945(9) 0.0189(8) 0.051 Uani
H(3) H -0.60440 0.03670 0.36349 0.090 Uiso
H(4) H -0.71488 -0.01968 0.21843 0.120 Uiso
H(5) H -0.62391 -0.06524 0.08641 0.128 Uiso
H(6) H -0.40169 -0.02980 0.08819 0.085 Uiso
H(71) H -0.30100 0.03145 0.41114 0.083 Uiso
H(72) H -0.41426 0.07082 0.45104 0.083 Uiso
H(73) H -0.31431 0.15469 0.40087 0.083 Uiso
H(12) H -0.01448 -0.02043 0.38056 0.073 Uiso
H(13) H 0.15203 -0.06095 0.46340 0.094 Uiso
H(14) H 0.18512 -0.23759 0.44396 0.093 Uiso
H(15) H 0.05145 -0.38473 0.34258 0.087 Uiso
H(16) H -0.11884 -0.34798 0.25774 0.070 Uiso
H(22) H -0.22829 -0.20347 0.44469 0.069 Uiso
H(23) H -0.39473 -0.26682 0.54368 0.090 Uiso
H(24) H -0.60241 -0.31972 0.48467 0.089 Uiso
H(25) H -0.65106 -0.29734 0.33083 0.086 Uiso
H(26) H -0.48792 -0.22609 0.23185 0.068 Uiso
H(32) H -0.34962 -0.38921 0.19578 0.058 Uiso
H(33) H -0.39458 -0.50256 0.05188 0.074 Uiso
H(34) H -0.33556 -0.42292 -0.08659 0.075 Uiso
H(35) H -0.21905 -0.23481 -0.08144 0.080 Uiso
H(36) H -0.17031 -0.11825 0.06260 0.059 Uiso
H(42) H 0.07237 0.40136 0.16301 0.060 Uiso
H(43) H 0.25658 0.49565 0.24773 0.071 Uiso
H(44) H 0.28558 0.47345 0.40791 0.078 Uiso
H(45) H 0.12588 0.35196 0.47963 0.081 Uiso
H(46) H -0.05521 0.24735 0.38943 0.069 Uiso
H(52) H -0.15933 0.42598 0.34944 0.068 Uiso
H(53) H -0.30789 0.51965 0.39656 0.087 Uiso
H(54) H -0.50947 0.45796 0.33211 0.082 Uiso
H(55) H -0.56565 0.31017 0.21333 0.084 Uiso
H(56) H -0.42024 0.21509 0.16476 0.071 Uiso
H(62) H -0.18132 0.42496 0.10718 0.082 Uiso
H(63) H -0.15923 0.46705 -0.04922 0.110 Uiso
H(64) H -0.11873 0.33439 -0.16335 0.093 Uiso
H(65) H -0.08600 0.16448 -0.12098 0.079 Uiso
H(66) H -0.10256 0.12467 0.03673 0.061 Uiso
loop_
_atom_type_symbol
_atom_type_scat_source
Pd
'International Tables for X-ray Crystallography (1974, Vol IV, Tables 2.2B and 2.3.1)'
Br
'International Tables for X-ray Crystallography (1974, Vol IV, Tables 2.2B and 2.3.1)'
B
'International Tables for X-ray Crystallography (1974, Vol IV, Tables 2.2B and 2.3.1)'
C
'International Tables for X-ray Crystallography (1974, Vol IV, Tables 2.2B and 2.3.1)'
H
'International Tables for X-ray Crystallography (1974, Vol IV, Tables 2.2B and 2.3.1)'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-2 1 -3
3 8 -5
5 7 -2
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Br(1) Pd(1) P(1) . . . 93.00(10) no
Br(1) Pd(1) P(2) . . . 89.80(10) no
Br(1) Pd(1) C(1) . . . 171.3(4) no
P(1) Pd(1) P(2) . . . 175.8(2) no
P(1) Pd(1) C(1) . . . 87.5(3) no
P(2) Pd(1) C(1) . . . 90.2(3) no
Pd(1) P(1) C(11) . . . 114.0(4) no
Pd(1) P(1) C(21) . . . 118.5(4) no
Pd(1) P(1) C(31) . . . 110.3(4) no
C(11) P(1) C(21) . . . 102.0(5) no
C(11) P(1) C(31) . . . 106.8(5) no
C(21) P(1) C(31) . . . 104.0(5) no
Pd(1) P(2) C(41) . . . 108.6(4) no
Pd(1) P(2) C(51) . . . 120.6(4) no
Pd(1) P(2) C(61) . . . 115.1(4) no
C(41) P(2) C(51) . . . 103.7(5) no
C(41) P(2) C(61) . . . 104.5(5) no
C(51) P(2) C(61) . . . 102.8(5) no
Pd(1) C(1) C(2) . . . 125.8(9) no
Pd(1) C(1) C(6) . . . 114.2(9) no
C(2) C(1) C(6) . . . 120.0(11) no
C(1) C(2) C(3) . . . 120.7(12) no
C(1) C(2) C(7) . . . 120.0(11) no
C(3) C(2) C(7) . . . 119.3(12) no
C(2) C(3) C(4) . . . 117.2(14) no
C(3) C(4) C(5) . . . 124.4(15) no
C(4) C(5) C(6) . . . 119.3(16) no
C(1) C(6) C(5) . . . 118.2(14) no
P(1) C(11) C(12) . . . 119.8(9) no
P(1) C(11) C(16) . . . 120.6(9) no
C(12) C(11) C(16) . . . 119.5(11) no
C(11) C(12) C(13) . . . 120.4(12) no
C(12) C(13) C(14) . . . 121.1(13) no
C(13) C(14) C(15) . . . 121.1(12) no
C(14) C(15) C(16) . . . 119.2(13) no
C(11) C(16) C(15) . . . 118.8(13) no
P(1) C(21) C(22) . . . 118.3(8) no
P(1) C(21) C(26) . . . 122.0(8) no
C(22) C(21) C(26) . . . 119.4(10) no
C(21) C(22) C(23) . . . 117.4(12) no
C(22) C(23) C(24) . . . 121.6(13) no
C(23) C(24) C(25) . . . 120.1(13) no
C(24) C(25) C(26) . . . 119.9(13) no
C(21) C(26) C(25) . . . 121.5(12) no
P(1) C(31) C(32) . . . 123.0(8) no
P(1) C(31) C(36) . . . 120.3(8) no
C(32) C(31) C(36) . . . 116.6(10) no
C(31) C(32) C(33) . . . 120.9(11) no
C(32) C(33) C(34) . . . 120.5(11) no
C(33) C(34) C(35) . . . 119.7(12) no
C(34) C(35) C(36) . . . 120.9(11) no
C(31) C(36) C(35) . . . 121.2(10) no
P(2) C(41) C(42) . . . 124.1(9) no
P(2) C(41) C(46) . . . 118.3(8) no
C(42) C(41) C(46) . . . 117.5(11) no
C(41) C(42) C(43) . . . 120.7(11) no
C(42) C(43) C(44) . . . 121.4(11) no
C(43) C(44) C(45) . . . 118.5(11) no
C(44) C(45) C(46) . . . 119.1(12) no
C(41) C(46) C(45) . . . 122.8(11) no
P(2) C(51) C(52) . . . 122.4(8) no
P(2) C(51) C(56) . . . 121.7(9) no
C(52) C(51) C(56) . . . 115.9(10) no
C(51) C(52) C(53) . . . 120.8(11) no
C(52) C(53) C(54) . . . 120.3(12) no
C(53) C(54) C(55) . . . 121.1(12) no
C(54) C(55) C(56) . . . 119.2(12) no
C(51) C(56) C(55) . . . 122.7(12) no
P(2) C(61) C(62) . . . 122.6(9) no
P(2) C(61) C(66) . . . 119.9(8) no
C(62) C(61) C(66) . . . 117.5(10) no
C(61) C(62) C(63) . . . 120.3(11) no
C(62) C(63) C(64) . . . 121.3(12) no
C(63) C(64) C(65) . . . 119.8(12) no
C(64) C(65) C(66) . . . 118.9(11) no
C(61) C(66) C(65) . . . 122.2(11) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd(1) Br(1) . . 2.524(2) no
Pd(1) P(1) . . 2.318(3) no
Pd(1) P(2) . . 2.322(3) no
Pd(1) C(1) . . 2.009(10) no
P(1) C(11) . . 1.838(11) no
P(1) C(21) . . 1.840(10) no
P(1) C(31) . . 1.803(11) no
P(2) C(41) . . 1.828(11) no
P(2) C(51) . . 1.834(10) no
P(2) C(61) . . 1.806(10) no
C(1) C(2) . . 1.366(15) no
C(1) C(6) . . 1.419(16) no
C(2) C(3) . . 1.418(16) no
C(2) C(7) . . 1.442(17) no
C(3) C(4) . . 1.36(3) no
C(4) C(5) . . 1.33(3) no
C(5) C(6) . . 1.42(2) no
C(11) C(12) . . 1.372(15) no
C(11) C(16) . . 1.397(15) no
C(12) C(13) . . 1.378(17) no
C(13) C(14) . . 1.316(19) no
C(14) C(15) . . 1.394(19) no
C(15) C(16) . . 1.399(16) no
C(21) C(22) . . 1.412(15) no
C(21) C(26) . . 1.361(14) no
C(22) C(23) . . 1.411(17) no
C(23) C(24) . . 1.37(2) no
C(24) C(25) . . 1.344(19) no
C(25) C(26) . . 1.398(16) no
C(31) C(32) . . 1.429(14) no
C(31) C(36) . . 1.384(14) no
C(32) C(33) . . 1.364(16) no
C(33) C(34) . . 1.381(17) no
C(34) C(35) . . 1.353(17) no
C(35) C(36) . . 1.386(15) no
C(41) C(42) . . 1.380(14) no
C(41) C(46) . . 1.366(15) no
C(42) C(43) . . 1.347(16) no
C(43) C(44) . . 1.397(17) no
C(44) C(45) . . 1.362(17) no
C(45) C(46) . . 1.377(16) no
C(51) C(52) . . 1.413(15) no
C(51) C(56) . . 1.372(15) no
C(52) C(53) . . 1.351(15) no
C(53) C(54) . . 1.338(18) no
C(54) C(55) . . 1.354(18) no
C(55) C(56) . . 1.348(16) no
C(61) C(62) . . 1.381(15) no
C(61) C(66) . . 1.388(15) no
C(62) C(63) . . 1.383(16) no
C(63) C(64) . . 1.373(19) no
C(64) C(65) . . 1.363(18) no
C(65) C(66) . . 1.394(16) no
