#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/50/4115032.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_4115032
loop_
_publ_author_name
'James P. Stambuli'
'Michael Bühl'
'John F. Hartwig'
_publ_section_title
;
 Synthesis, Characterization, and Reactivity of Monomeric, Arylpalladium
 Halide Complexes with a Hindered Phosphine as the Only Dative Ligand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9346
_journal_page_last               9347
_journal_paper_doi               10.1021/ja0264394
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         'C24 H38 Br P Pd '
_chemical_formula_sum            'C24 H38 Br P Pd'
_chemical_formula_weight         543.84
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             'Fri May 18 13:32:14 2002'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 112.187(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2935(5)
_cell_length_b                   18.229(1)
_cell_length_c                   12.0440(5)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    183.2
_cell_measurement_theta_max      0.0
_cell_measurement_theta_min      0.0
_cell_volume                     2295.90(19)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      183.2
_diffrn_measurement_device       unknown
_diffrn_measurement_method       'omega scans with profile analysis'
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.00
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4214
_diffrn_reflns_theta_max         25.03
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.631
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       plate
_exptl_crystal_F_000             1112.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.360
_refine_ls_goodness_of_fit_obs   1.434
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         2992
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_obs          0.0391
_refine_ls_shift/esd_max         0.0418
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0363
_refine_ls_wR_factor_obs         0.0325
_reflns_number_observed          2992
_reflns_number_total             4214
_reflns_observed_criterion       I>2u(I)
_cod_data_source_file            ja0264394_s3_1.cif
_cod_data_source_block           complex
_cod_original_cell_volume        2295.8(2)
_cod_original_sg_symbol_H-M      'P 21/c     '
_cod_original_formula_sum        'C24 H38 Br P Pd '
_cod_database_code               4115032
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'   -x,1/2+y,1/2-z'
'   -x,   -y,   -z'
'   +x,1/2-y,1/2+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
Pd(1) 0.13906(3) 0.07426(2) 0.12837(3) 0.0274(1) Uij
Br(1) 0.08462(4) 0.07013(3) -0.09047(4) 0.0365(1) Uij
P(1) 0.1754(1) 0.11494(6) 0.31889(9) 0.0258(3) Uij
C(1) 0.2922(4) 0.0128(2) 0.1581(3) 0.028(1) Uij
C(2) 0.3931(4) 0.0386(2) 0.1292(4) 0.034(1) Uij
C(3) 0.4933(4) -0.0080(3) 0.1393(4) 0.037(1) Uij
C(4) 0.4932(4) -0.0797(3) 0.1751(4) 0.041(2) Uij
C(5) 0.3917(5) -0.1058(3) 0.2002(4) 0.037(1) Uij
C(6) 0.2912(4) -0.0599(2) 0.1919(4) 0.030(1) Uij
C(7) 0.0077(4) 0.1531(2) 0.2821(3) 0.025(1) Uij
C(8) -0.0823(4) 0.0936(2) 0.2967(3) 0.026(1) Uij
C(9) -0.2214(4) 0.1212(2) 0.2543(3) 0.028(1) Uij
C(10) -0.2696(4) 0.1385(2) 0.1207(4) 0.035(1) Uij
C(11) -0.1843(4) 0.1981(2) 0.1019(3) 0.032(1) Uij
C(12) -0.1893(4) 0.2674(2) 0.1722(4) 0.039(1) Uij
C(13) -0.1440(4) 0.2486(2) 0.3068(4) 0.033(1) Uij
C(14) -0.2287(4) 0.1886(2) 0.3245(3) 0.032(1) Uij
C(15) -0.0453(4) 0.1716(3) 0.1451(4) 0.028(1) Uij
C(16) -0.0046(4) 0.2217(2) 0.3521(3) 0.030(1) Uij
C(17) 0.2166(4) 0.0506(2) 0.4519(3) 0.029(1) Uij
C(18) 0.1440(4) -0.0211(2) 0.4121(3) 0.032(1) Uij
C(19) 0.3595(4) 0.0309(3) 0.4952(4) 0.042(2) Uij
C(20) 0.1918(4) 0.0828(2) 0.5593(4) 0.034(1) Uij
C(21) 0.2947(4) 0.1946(2) 0.3565(4) 0.035(1) Uij
C(22) 0.2450(5) 0.2512(3) 0.2549(4) 0.048(2) Uij
C(23) 0.4231(4) 0.1669(3) 0.3531(4) 0.051(2) Uij
C(24) 0.3235(4) 0.2325(3) 0.4765(4) 0.038(1) Uij
H(17) 0.012(3) 0.208(2) 0.131(3) 0.015(10) Uij
H(18) -0.048(3) 0.132(2) 0.100(3) 0.013(10) Uij
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 96 0.003 0.002 'International Tables'
H 0 152 0.000 0.000 'International Tables'
P 0 4 0.102 0.094 'International Tables'
Br 0 4 -0.290 2.459 'International Tables'
Pd 0 4 -0.999 1.007 'International Tables'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
Br(1) Pd(1) P(1) 162.61(3) yes
Br(1) Pd(1) C(1) 91.4(1) yes
P(1) Pd(1) C(1) 100.8(1) yes
Pd(1) P(1) C(7) 95.6(1) yes
Pd(1) P(1) C(17) 122.6(1) yes
Pd(1) P(1) C(21) 109.0(1) yes
C(7) P(1) C(17) 109.1(2) yes
C(7) P(1) C(21) 109.1(2) yes
C(17) P(1) C(21) 110.1(2) yes
Pd(1) C(1) C(2) 120.4(3) yes
Pd(1) C(1) C(6) 119.4(3) yes
C(2) C(1) C(6) 119.6(4) yes
C(1) C(2) C(3) 119.4(4) yes
C(2) C(3) C(4) 120.8(4) yes
C(3) C(4) C(5) 119.8(4) yes
C(4) C(5) C(6) 120.3(4) yes
C(1) C(6) C(5) 120.1(4) yes
P(1) C(7) C(8) 110.9(3) yes
P(1) C(7) C(15) 106.0(3) yes
P(1) C(7) C(16) 117.1(3) yes
C(8) C(7) C(15) 105.4(3) yes
C(8) C(7) C(16) 108.0(3) yes
C(15) C(7) C(16) 108.9(3) yes
C(7) C(8) C(9) 111.5(3) yes
C(8) C(9) C(10) 109.2(3) yes
C(8) C(9) C(14) 110.1(3) yes
C(10) C(9) C(14) 110.4(3) yes
C(9) C(10) C(11) 108.1(3) yes
C(10) C(11) C(12) 110.4(3) yes
C(10) C(11) C(15) 110.3(4) yes
C(12) C(11) C(15) 108.6(4) yes
C(11) C(12) C(13) 109.3(3) yes
C(12) C(13) C(14) 109.3(4) yes
C(12) C(13) C(16) 109.4(3) yes
C(14) C(13) C(16) 109.5(3) yes
C(9) C(14) C(13) 109.7(3) yes
C(7) C(15) C(11) 111.1(3) yes
C(7) C(16) C(13) 110.9(3) yes
P(1) C(17) C(18) 109.5(3) yes
P(1) C(17) C(19) 108.8(3) yes
P(1) C(17) C(20) 114.2(3) yes
C(18) C(17) C(19) 106.1(4) yes
C(18) C(17) C(20) 110.2(3) yes
C(19) C(17) C(20) 107.7(3) yes
P(1) C(21) C(22) 108.0(3) yes
P(1) C(21) C(23) 109.2(3) yes
P(1) C(21) C(24) 116.6(3) yes
C(22) C(21) C(23) 105.2(4) yes
C(22) C(21) C(24) 109.5(4) yes
C(23) C(21) C(24) 107.8(3) yes
C(7) C(15) H(17) 108(2) yes
C(7) C(15) H(18) 112(2) yes
C(11) C(15) H(17) 112(2) yes
C(11) C(15) H(18) 104(2) yes
H(17) C(15) H(18) 108(3) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Pd(1) Br(1) 2.4711(5) yes
Pd(1) P(1) 2.296(1) yes
Pd(1) C(1) 1.977(4) yes
P(1) C(7) 1.906(4) yes
P(1) C(17) 1.896(4) yes
P(1) C(21) 1.915(4) yes
C(1) C(2) 1.393(6) yes
C(1) C(6) 1.388(6) yes
C(2) C(3) 1.383(6) yes
C(3) C(4) 1.377(6) yes
C(4) C(5) 1.376(6) yes
C(5) C(6) 1.382(6) yes
C(7) C(8) 1.541(5) yes
C(7) C(15) 1.565(5) yes
C(7) C(16) 1.543(5) yes
C(8) C(9) 1.542(5) yes
C(9) C(10) 1.525(5) yes
C(9) C(14) 1.511(6) yes
C(10) C(11) 1.526(6) yes
C(11) C(12) 1.533(6) yes
C(11) C(15) 1.533(6) yes
C(12) C(13) 1.543(5) yes
C(13) C(14) 1.520(6) yes
C(13) C(16) 1.539(6) yes
C(17) C(18) 1.522(6) yes
C(17) C(19) 1.540(6) yes
C(17) C(20) 1.539(6) yes
C(21) C(22) 1.536(6) yes
C(21) C(23) 1.549(6) yes
C(21) C(24) 1.523(6) yes
C(15) H(17) 0.99(3) yes
C(15) H(18) 0.90(3) yes
