#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:50:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179734 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/30/7003090.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_7003090
loop_
_publ_author_name
'Barnes, Nicholas A.'
'Brisdon, Alan K.'
'Brown, F. R. William'
'Cross, Wendy I.'
'Herbert, Christopher J.'
'Pritchard, Robin G.'
'Sadiq, Ghazala'
_publ_section_title
;
 The coordination chemistry of perfluorovinyl substituted phosphine
 ligands, a crystallographic and spectroscopic study.
 Co-crystallisation of both cis- and trans-isomers of
 [PtCl2{PiPr2(CFCF2)}2] within the same unit cell
;
_journal_issue                   1
_journal_name_full               'Dalton Transactions'
_journal_page_first              101
_journal_paper_doi               10.1039/b711825b
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C20 H10 Br2 F12 P2 Pd1'
_chemical_formula_sum            'C20 H10 Br2 F12 P2 Pd'
_chemical_formula_weight         806.44
_chemical_name_systematic
;
bis(phenylbisperfluorovinylphosphine)palladium(II) bromide
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2007-07-03T23:36:53-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                109.062(10)
_cell_angle_beta                 102.91(2)
_cell_angle_gamma                99.26(2)
_cell_formula_units_Z            1
_cell_length_a                   9.105(2)
_cell_length_b                   10.0130(10)
_cell_length_c                   7.8700(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      36
_cell_measurement_theta_min      25
_cell_measurement_wavelength     1.5418
_cell_volume                     639.4(2)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2191
_diffrn_reflns_theta_full        64.99
_diffrn_reflns_theta_max         64.99
_diffrn_reflns_theta_min         6.81
_exptl_absorpt_coefficient_mu    11.628
_exptl_absorpt_correction_T_max  0.2744
_exptl_absorpt_correction_T_min  0.1091
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was 4
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.775
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.14
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.07
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.07
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1024P)²+0.9402P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.1745
_reflns_number_gt                1474
_reflns_number_total             2048
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b711825b.txt
_cod_data_source_block           PdBrPhpfv2
_cod_original_cell_volume        639.34(17)
_cod_database_code               7003090
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.5 0 0 0.0541(3) Uani 1 2 d S . .
Br1 Br 0.40193(13) 0.02317(13) 0.26525(16) 0.0805(4) Uani 1 1 d . . .
P1 P 0.6937(3) 0.2101(3) 0.1866(4) 0.0610(6) Uani 1 1 d . . .
C1 C 0.7998(11) 0.2087(12) 0.4083(15) 0.071(3) Uani 1 1 d . . .
C2 C 0.8205(12) 0.0938(17) 0.4415(19) 0.084(3) Uani 1 1 d . . .
C3 C 0.8539(13) 0.2514(14) 0.0925(19) 0.084(3) Uani 1 1 d . . .
C4 C 0.9721(16) 0.207(2) 0.098(2) 0.122(6) Uani 1 1 d . . .
C5 C 0.6289(11) 0.3767(10) 0.2419(15) 0.066(2) Uani 1 1 d . . .
C6 C 0.4726(13) 0.3669(12) 0.1798(18) 0.079(3) Uani 1 1 d . . .
H6 H 0.401 0.2764 0.1149 0.095 Uiso 1 1 calc R . .
C7 C 0.4243(16) 0.4945(15) 0.216(2) 0.101(4) Uani 1 1 d . . .
H7 H 0.3188 0.4891 0.1738 0.121 Uiso 1 1 calc R . .
C8 C 0.5254(19) 0.6260(15) 0.311(2) 0.105(4) Uani 1 1 d . . .
H8 H 0.4901 0.7104 0.3343 0.126 Uiso 1 1 calc R . .
C9 C 0.678(2) 0.6346(15) 0.371(2) 0.118(5) Uani 1 1 d . . .
H9 H 0.7489 0.7255 0.438 0.142 Uiso 1 1 calc R . .
C10 C 0.7314(16) 0.5096(13) 0.334(2) 0.099(4) Uani 1 1 d . . .
H10 H 0.8375 0.5165 0.3734 0.118 Uiso 1 1 calc R . .
F1 F 0.8693(8) 0.3399(8) 0.5516(11) 0.109(2) Uani 1 1 d . . .
F2 F 0.9056(9) 0.0972(11) 0.6046(12) 0.119(3) Uani 1 1 d . . .
F3 F 0.7662(10) -0.0371(9) 0.3270(13) 0.114(3) Uani 1 1 d . . .
F4 F 0.8301(12) 0.3447(12) -0.0128(16) 0.141(3) Uani 1 1 d . . .
F5 F 1.0765(10) 0.2488(15) 0.0115(15) 0.183(6) Uani 1 1 d . . .
F6 F 1.0051(13) 0.1264(17) 0.1831(17) 0.166(5) 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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 '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
P1 Pd1 P1 180.00(11) 2_655 . ?
P1 Pd1 Br1 91.44(7) 2_655 . ?
P1 Pd1 Br1 88.56(7) . . ?
P1 Pd1 Br1 88.56(7) 2_655 2_655 ?
P1 Pd1 Br1 91.44(7) . 2_655 ?
Br1 Pd1 Br1 180.00(5) . 2_655 ?
C1 P1 C5 106.1(5) . . ?
C1 P1 C3 100.5(5) . . ?
C5 P1 C3 103.0(5) . . ?
C1 P1 Pd1 114.4(4) . . ?
C5 P1 Pd1 114.9(3) . . ?
C3 P1 Pd1 116.3(4) . . ?
C6 C5 C10 119.8(10) . . ?
C10 C5 P1 121.5(9) . . ?
C6 C5 P1 118.6(7) . . ?
C5 C6 C7 118.4(11) . . ?
C5 C6 H6 120.8 . . ?
C6 C6 H6 120.8 . . ?
C8 C7 C6 121.8(13) . . ?
C8 C7 H7 119.1 . . ?
C6 C7 H7 119.1 . . ?
C7 C8 C9 119.4(13) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
C8 C9 C10 120.4(13) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C5 C10 C9 120.1(13) . . ?
C5 C10 H10 120 . . ?
C9 C10 H10 120 . . ?
C2 C1 F1 116.8(10) . . ?
C2 C1 P1 125.7(10) . . ?
F1 C1 P1 117.4(8) . . ?
F3 C2 C1 126.3(11) . . ?
F3 C2 F2 109.6(11) . . ?
C1 C2 F2 124.1(14) . . ?
C4 C3 F4 116.6(14) . . ?
C4 C3 P1 129.9(14) . . ?
F4 C3 P1 113.4(8) . . ?
C3 C4 F6 122.7(16) . . ?
C3 C4 F5 120(2) . . ?
F6 C4 F5 117.0(14) . . ?
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 P1 2.307(2) 2_655 ?
Pd1 P1 2.307(2) . ?
Pd1 Br1 2.4067(11) . ?
Pd1 Br1 2.4067(11) 2_655 ?
P1 C1 1.802(10) . ?
P1 C5 1.810(10) . ?
P1 C3 1.826(11) . ?
C5 C10 1.355(15) . ?
C5 C6 1.374(14) . ?
C6 C7 1.380(16) . ?
C6 H6 0.93 . ?
C7 C8 1.34(2) . ?
C7 H7 0.93 . ?
C8 C9 1.35(2) . ?
C8 H8 0.93 . ?
C9 C10 1.380(19) . ?
C9 H9 0.93 . ?
C10 H10 0.93 . ?
C1 C2 1.293(17) . ?
C1 F1 1.357(13) . ?
C2 F3 1.263(16) . ?
C2 F2 1.329(13) . ?
C3 C4 1.226(19) . ?
C3 F4 1.448(15) . ?
C4 F6 1.24(2) . ?
C4 F5 1.375(18) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 Pd1 P1 C1 -14E1(10) 2_655 . . . ?
Br1 Pd1 P1 C1 51.3(4) . . . . ?
Br1 Pd1 P1 C1 -128.7(4) 2_655 . . . ?
P1 Pd1 P1 C5 10E1(10) 2_655 . . . ?
Br1 Pd1 P1 C5 -71.8(4) . . . . ?
Br1 Pd1 P1 C5 108.2(4) 2_655 . . . ?
P1 Pd1 P1 C3 -2E1(10) 2_655 . . . ?
Br1 Pd1 P1 C3 167.8(5) . . . . ?
Br1 Pd1 P1 C3 -12.2(5) 2_655 . . . ?
C1 P1 C5 C10 59.1(12) . . . . ?
C3 P1 C5 C10 -46.0(12) . . . . ?
Pd1 P1 C5 C10 -173.5(10) . . . . ?
C1 P1 C5 C6 -124.1(10) . . . . ?
C3 P1 C5 C6 130.8(10) . . . . ?
Pd1 P1 C5 C6 3.3(11) . . . . ?
C10 C5 C6 C7 -0.7(19) . . . . ?
P1 C5 C6 C7 -177.6(10) . . . . ?
C5 C6 C7 C8 0(2) . . . . ?
C6 C7 C8 C9 0(3) . . . . ?
C7 C8 C9 C10 1(3) . . . . ?
C6 C5 C10 C9 2(2) . . . . ?
P1 C5 C10 C9 178.7(12) . . . . ?
C8 C9 C10 C5 -2(3) . . . . ?
C5 P1 C1 C2 155.4(10) . . . . ?
C3 P1 C1 C2 -97.7(11) . . . . ?
Pd1 P1 C1 C2 27.6(11) . . . . ?
C5 P1 C1 F1 -27.3(9) . . . . ?
C3 P1 C1 F1 79.6(9) . . . . ?
Pd1 P1 C1 F1 -155.0(7) . . . . ?
F1 C1 C2 F3 -179.8(10) . . . . ?
P1 C1 C2 F3 -2.4(18) . . . . ?
F1 C1 C2 F2 -0.6(17) . . . . ?
P1 C1 C2 F2 176.8(8) . . . . ?
C1 P1 C3 C4 40.0(16) . . . . ?
C5 P1 C3 C4 149.4(15) . . . . ?
Pd1 P1 C3 C4 -84.1(16) . . . . ?
C1 P1 C3 F4 -143.8(9) . . . . ?
C5 P1 C3 F4 -34.3(10) . . . . ?
Pd1 P1 C3 F4 92.2(9) . . . . ?
F4 C3 C4 F6 -179.8(15) . . . . ?
P1 C3 C4 F6 -4(3) . . . . ?
F4 C3 C4 F5 2(2) . . . . ?
P1 C3 C4 F5 177.7(11) . . . . ?
