#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:45:54 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179763 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/59/7005912.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_7005912
loop_
_publ_author_name
'Albéniz, Ana C'
'Espinet, Pablo'
'Martín-Ruiz, Blanca'
_publ_section_title
;
 Pd-H elimination reactions in palladium(II) allylic complexes.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3710
_journal_page_last               3714
_journal_paper_doi               10.1039/b706817d
_journal_year                    2007
_chemical_formula_sum            'C15 H17 Br F5 P Pd'
_chemical_formula_weight         509.57
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 102.445(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.1018(18)
_cell_length_b                   21.654(5)
_cell_length_c                   12.220(3)
_cell_measurement_temperature    566(2)
_cell_volume                     1835.1(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      566(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0702
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8553
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    3.315
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.431812
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.432
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         2643
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0944P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1612
_reflns_number_gt                1509
_reflns_number_total             2643
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b706817d.txt
_cod_data_source_block           bm552
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7005912
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -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 0.16990(11) 0.45576(4) 0.72529(6) 0.0589(3) Uani 1 1 d . . .
C1 C 0.1147(15) 0.4886(6) 0.8876(8) 0.069(3) Uani 1 1 d . . .
H1 H 0.1015 0.5331 0.8991 0.083 Uiso 1 1 calc R . .
C2 C -0.0435(14) 0.4557(6) 0.8220(9) 0.075(3) Uani 1 1 d . . .
H2 H -0.1689 0.4756 0.7949 0.090 Uiso 1 1 calc R . .
C3 C -0.0110(13) 0.3954(6) 0.7949(8) 0.067(3) Uani 1 1 d . . .
H3 H -0.1153 0.3750 0.7416 0.080 Uiso 1 1 calc R . .
C4 C 0.1234(15) 0.3538(5) 0.8754(8) 0.069(3) Uani 1 1 d . . .
H4A H 0.2289 0.3408 0.8419 0.083 Uiso 1 1 calc R . .
H4B H 0.0543 0.3172 0.8904 0.083 Uiso 1 1 calc R . .
C5 C 0.2047(13) 0.3883(5) 0.9867(7) 0.058(3) Uani 1 1 d . . .
H5 H 0.0984 0.3921 1.0258 0.069 Uiso 1 1 calc R . .
C6 C 0.2701(14) 0.4528(4) 0.9684(8) 0.062(3) Uani 1 1 d . . .
H6A H 0.3859 0.4509 0.9385 0.074 Uiso 1 1 calc R . .
H6B H 0.3015 0.4743 1.0396 0.074 Uiso 1 1 calc R . .
P1 P 0.2179(4) 0.39952(14) 0.5747(2) 0.0649(8) Uani 1 1 d . . .
Br1 Br 0.40648(19) 0.53751(6) 0.70404(10) 0.0869(5) Uani 1 1 d . . .
C13 C 0.1815(17) 0.4412(6) 0.4465(8) 0.093(4) Uani 1 1 d . . .
H13A H 0.2463 0.4205 0.3957 0.140 Uiso 1 1 calc R . .
H13B H 0.2327 0.4822 0.4607 0.140 Uiso 1 1 calc R . .
H13C H 0.0461 0.4435 0.4140 0.140 Uiso 1 1 calc R . .
C14 C 0.083(3) 0.3302(7) 0.5400(13) 0.156(8) Uani 1 1 d . . .
H14A H -0.0421 0.3399 0.4953 0.234 Uiso 1 1 calc R . .
H14B H 0.0684 0.3098 0.6075 0.234 Uiso 1 1 calc R . .
H14C H 0.1495 0.3034 0.4985 0.234 Uiso 1 1 calc R . .
C15 C 0.4662(18) 0.3754(7) 0.5921(11) 0.119(5) Uani 1 1 d . . .
H15A H 0.4736 0.3410 0.5436 0.179 Uiso 1 1 calc R . .
H15B H 0.5154 0.3634 0.6685 0.179 Uiso 1 1 calc R . .
H15C H 0.5416 0.4090 0.5732 0.179 Uiso 1 1 calc R . .
C7 C 0.3604(15) 0.3504(5) 1.0619(8) 0.062(3) Uani 1 1 d . . .
C8 C 0.344(2) 0.3325(5) 1.1687(10) 0.079(3) Uani 1 1 d . . .
C9 C 0.489(3) 0.3002(6) 1.2394(11) 0.103(5) Uani 1 1 d . . .
C10 C 0.655(3) 0.2850(6) 1.2045(15) 0.115(6) Uani 1 1 d . . .
C11 C 0.6794(19) 0.3037(6) 1.1056(15) 0.092(4) Uani 1 1 d . . .
C12 C 0.5360(17) 0.3363(5) 1.0319(10) 0.076(3) Uani 1 1 d . . .
F8 F 0.1843(12) 0.3457(4) 1.2050(5) 0.105(2) Uani 1 1 d . . .
F9 F 0.4664(16) 0.2829(4) 1.3395(6) 0.156(4) Uani 1 1 d . . .
F10 F 0.7959(15) 0.2545(4) 1.2722(8) 0.174(4) Uani 1 1 d . . .
F11 F 0.8400(13) 0.2910(4) 1.0663(9) 0.146(3) Uani 1 1 d . . .
F12 F 0.5662(9) 0.3548(3) 0.9323(6) 0.095(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 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Pd1 C3 37.9(4) . . ?
C2 Pd1 C1 38.2(4) . . ?
C3 Pd1 C1 66.6(4) . . ?
C2 Pd1 P1 134.2(4) . . ?
C3 Pd1 P1 101.6(3) . . ?
C1 Pd1 P1 166.6(3) . . ?
C2 Pd1 Br1 129.7(4) . . ?
C3 Pd1 Br1 162.5(3) . . ?
C1 Pd1 Br1 96.8(3) . . ?
P1 Pd1 Br1 94.22(8) . . ?
C2 C1 C6 118.9(10) . . ?
C2 C1 Pd1 66.8(6) . . ?
C6 C1 Pd1 100.0(6) . . ?
C3 C2 C1 117.2(9) . . ?
C3 C2 Pd1 71.9(6) . . ?
C1 C2 Pd1 75.0(6) . . ?
C2 C3 C4 121.5(9) . . ?
C2 C3 Pd1 70.2(6) . . ?
C4 C3 Pd1 105.9(6) . . ?
C3 C4 C5 110.4(9) . . ?
C6 C5 C7 112.6(8) . . ?
C6 C5 C4 112.6(8) . . ?
C7 C5 C4 110.8(8) . . ?
C5 C6 C1 111.4(9) . . ?
C13 P1 C14 104.5(7) . . ?
C13 P1 C15 101.7(6) . . ?
C14 P1 C15 104.2(8) . . ?
C13 P1 Pd1 114.8(4) . . ?
C14 P1 Pd1 118.2(5) . . ?
C15 P1 Pd1 111.7(4) . . ?
C8 C7 C12 116.4(10) . . ?
C8 C7 C5 121.3(10) . . ?
C12 C7 C5 122.1(10) . . ?
F8 C8 C9 118.4(13) . . ?
F8 C8 C7 120.2(10) . . ?
C9 C8 C7 121.4(14) . . ?
F9 C9 C10 120.2(16) . . ?
F9 C9 C8 119.7(18) . . ?
C10 C9 C8 120.1(14) . . ?
C11 C10 F10 119(2) . . ?
C11 C10 C9 120.0(14) . . ?
F10 C10 C9 120.4(19) . . ?
C10 C11 F11 123.2(15) . . ?
C10 C11 C12 121.6(15) . . ?
F11 C11 C12 115.2(15) . . ?
F12 C12 C11 119.9(13) . . ?
F12 C12 C7 119.7(9) . . ?
C11 C12 C7 120.4(13) . . ?
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 C2 2.113(10) . ?
Pd1 C3 2.134(10) . ?
Pd1 C1 2.220(10) . ?
Pd1 P1 2.292(3) . ?
Pd1 Br1 2.4924(15) . ?
C1 C2 1.422(15) . ?
C1 C6 1.525(13) . ?
C2 C3 1.380(14) . ?
C3 C4 1.512(13) . ?
C4 C5 1.550(12) . ?
C5 C6 1.504(12) . ?
C5 C7 1.517(13) . ?
P1 C13 1.778(11) . ?
P1 C14 1.783(12) . ?
P1 C15 1.808(11) . ?
C7 C8 1.392(15) . ?
C7 C12 1.406(15) . ?
C8 F8 1.332(14) . ?
C8 C9 1.385(18) . ?
C9 F9 1.323(15) . ?
C9 C10 1.38(2) . ?
C10 C11 1.32(2) . ?
C10 F10 1.329(15) . ?
C11 F11 1.358(16) . ?
C11 C12 1.397(17) . ?
C12 F12 1.342(13) . ?
