#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/07/7050775.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_7050775
loop_
_publ_author_name
'Inés García-Seijo, M.'
'Habtemariam, Abraha'
'Parsons, Simon'
'Gould, R. O.'
'Esther García-Fernández, M.'
_publ_section_title
;
 Reactivity of a cationic square-planar palladium(II) chloro complex
 containing bis[2-(diphenylphosphino)ethyl]amine: chloro substitutions
 by anionic ligands and formation of neutral digold(I) compounds
 possessing linear PAuX fragments. The X-Ray crystal structure of
 Au2[Ph2P(CH2)2N(NO)(CH2)2PPh2]Cl2
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              636
_journal_paper_doi               10.1039/b109675n
_journal_volume                  26
_journal_year                    2002
_chemical_formula_moiety         '[PdBr(Ph2PCH2CH2NHCH2CH2PPh2)]+Br-.Me2CO'
_chemical_formula_sum            'C31 H35 Br2 N O P2 Pd'
_chemical_formula_weight         765.76
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                114.823(13)
_cell_angle_beta                 101.696(19)
_cell_angle_gamma                98.816(17)
_cell_formula_units_Z            2
_cell_length_a                   11.722(4)
_cell_length_b                   12.209(4)
_cell_length_c                   12.640(4)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      12
_cell_volume                     1548.8(9)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    DIRDIF
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_method       Omega-theta'
_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  0.0833
_diffrn_reflns_av_sigmaI/netI    0.0686
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6158
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         2.65
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.307
_exptl_absorpt_correction_T_max  0.819
_exptl_absorpt_correction_T_min  0.532
_exptl_absorpt_correction_type   'Optimised numerical'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.237
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5495
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0585P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1104
_reflns_number_gt                3865
_reflns_number_total             5495
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b109675n.txt
_cod_data_source_block           pdinbr
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1548.8(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7050775
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 0.23820(4) 0.10499(4) 0.27978(4) 0.01735(14) Uani 1 1 d . . .
Br1 Br 0.02782(5) 0.08496(6) 0.19232(6) 0.02324(17) Uani 1 1 d . . .
P1 P 0.20927(16) -0.08957(16) 0.27129(15) 0.0253(4) Uani 1 1 d . . .
C11 C 0.1633(7) -0.2242(6) 0.1205(6) 0.0319(17) Uani 1 1 d . . .
C12 C 0.1886(9) -0.3364(7) 0.1074(7) 0.053(3) Uani 1 1 d . . .
H12 H 0.2329 -0.3419 0.1760 0.064 Uiso 1 1 calc R . .
C13 C 0.1475(10) -0.4413(7) -0.0090(7) 0.063(3) Uani 1 1 d . . .
H13 H 0.1632 -0.5185 -0.0188 0.076 Uiso 1 1 calc R . .
C14 C 0.0850(8) -0.4332(7) -0.1080(7) 0.047(2) Uani 1 1 d . . .
H14 H 0.0580 -0.5047 -0.1861 0.057 Uiso 1 1 calc R . .
C15 C 0.0609(7) -0.3218(6) -0.0954(6) 0.0350(17) Uani 1 1 d . . .
H15 H 0.0176 -0.3169 -0.1647 0.042 Uiso 1 1 calc R . .
C16 C 0.1003(6) -0.2164(6) 0.0195(6) 0.0268(15) Uani 1 1 d . . .
H16 H 0.0840 -0.1397 0.0284 0.032 Uiso 1 1 calc R . .
C21 C 0.1130(6) -0.1289(6) 0.3522(6) 0.0257(15) Uani 1 1 d . . .
C22 C -0.0020(7) -0.2111(6) 0.2890(6) 0.0329(17) Uani 1 1 d . . .
H22 H -0.0283 -0.2499 0.2023 0.040 Uiso 1 1 calc R . .
C23 C -0.0788(8) -0.2374(6) 0.3507(7) 0.0381(18) Uani 1 1 d . . .
H23 H -0.1567 -0.2945 0.3066 0.046 Uiso 1 1 calc R . .
C24 C -0.0405(7) -0.1791(6) 0.4780(6) 0.0334(17) Uani 1 1 d . . .
H24 H -0.0924 -0.1959 0.5213 0.040 Uiso 1 1 calc R . .
C25 C 0.0736(7) -0.0966(6) 0.5411(6) 0.0348(18) Uani 1 1 d . . .
H25 H 0.1001 -0.0582 0.6277 0.042 Uiso 1 1 calc R . .
C26 C 0.1492(7) -0.0694(6) 0.4796(6) 0.0310(17) Uani 1 1 d . . .
H26 H 0.2259 -0.0100 0.5240 0.037 Uiso 1 1 calc R . .
C2 C 0.3628(7) -0.0796(7) 0.3496(6) 0.0362(19) Uani 1 1 d . . .
H2A H 0.3740 -0.0464 0.4383 0.043 Uiso 1 1 calc R . .
H2B H 0.3771 -0.1638 0.3179 0.043 Uiso 1 1 calc R . .
C3 C 0.4502(7) 0.0062(7) 0.3275(6) 0.040(2) Uani 1 1 d . . .
H3A H 0.5336 0.0209 0.3766 0.048 Uiso 1 1 calc R . .
H3B H 0.4467 -0.0328 0.2402 0.048 Uiso 1 1 calc R . .
N4 N 0.4177(5) 0.1274(5) 0.3624(5) 0.0280(13) Uani 1 1 d . . .
H4 H 0.4259 0.1602 0.4454 0.034 Uiso 1 1 calc R . .
C5 C 0.5032(6) 0.2210(7) 0.3513(6) 0.0359(19) Uani 1 1 d . . .
H5A H 0.5033 0.1900 0.2653 0.043 Uiso 1 1 calc R . .
H5B H 0.5860 0.2363 0.4020 0.043 Uiso 1 1 calc R . .
C6 C 0.4642(6) 0.3421(6) 0.3940(6) 0.0320(17) Uani 1 1 d . . .
H6A H 0.5161 0.4045 0.3810 0.038 Uiso 1 1 calc R . .
H6B H 0.4714 0.3778 0.4821 0.038 Uiso 1 1 calc R . .
P7 P 0.30647(14) 0.30353(15) 0.30432(14) 0.0218(4) Uani 1 1 d . . .
C31 C 0.3120(6) 0.3171(6) 0.1684(6) 0.0283(15) Uani 1 1 d . . .
C32 C 0.3881(7) 0.4204(7) 0.1757(6) 0.0394(19) Uani 1 1 d . . .
H32 H 0.4346 0.4873 0.2536 0.047 Uiso 1 1 calc R . .
C33 C 0.3973(7) 0.4274(8) 0.0724(7) 0.051(2) Uani 1 1 d . . .
H33 H 0.4492 0.4991 0.0786 0.061 Uiso 1 1 calc R . .
C34 C 0.3297(7) 0.3282(8) -0.0432(7) 0.048(2) Uani 1 1 d . . .
H34 H 0.3373 0.3315 -0.1152 0.058 Uiso 1 1 calc R . .
C35 C 0.2529(7) 0.2268(7) -0.0510(6) 0.0366(18) Uani 1 1 d . . .
H35 H 0.2055 0.1611 -0.1290 0.044 Uiso 1 1 calc R . .
C36 C 0.2432(6) 0.2184(6) 0.0532(6) 0.0299(16) Uani 1 1 d . . .
H36 H 0.1907 0.1468 0.0467 0.036 Uiso 1 1 calc R . .
C41 C 0.2460(5) 0.4257(5) 0.3953(5) 0.0199(13) Uani 1 1 d . . .
C42 C 0.2384(6) 0.4374(6) 0.5080(6) 0.0282(15) Uani 1 1 d . . .
H42 H 0.2683 0.3844 0.5376 0.034 Uiso 1 1 calc R . .
C43 C 0.1875(6) 0.5257(6) 0.5763(6) 0.0334(17) Uani 1 1 d . . .
H43 H 0.1809 0.5315 0.6520 0.040 Uiso 1 1 calc R . .
C44 C 0.1459(6) 0.6059(6) 0.5374(6) 0.0313(16) Uani 1 1 d . . .
H44 H 0.1123 0.6672 0.5868 0.038 Uiso 1 1 calc R . .
C45 C 0.1529(7) 0.5973(6) 0.4262(6) 0.0361(18) Uani 1 1 d . . .
H45 H 0.1234 0.6519 0.3987 0.043 Uiso 1 1 calc R . .
C46 C 0.2036(7) 0.5081(6) 0.3548(6) 0.0335(17) Uani 1 1 d . . .
H46 H 0.2097 0.5026 0.2790 0.040 Uiso 1 1 calc R . .
Br2 Br -0.41031(7) -0.25405(7) 0.35338(6) 0.0340(2) Uani 1 1 d . . .
C1S C 0.5955(8) 0.2123(9) 0.0427(8) 0.065(3) Uani 1 1 d . . .
H1S1 H 0.5612 0.2016 -0.0396 0.098 Uiso 1 1 calc R . .
H1S2 H 0.6649 0.2865 0.0877 0.098 Uiso 1 1 calc R . .
H1S3 H 0.5340 0.2228 0.0857 0.098 Uiso 1 1 calc R . .
O1S O 0.6125(5) 0.0058(6) -0.0632(5) 0.0546(16) Uani 1 1 d . . .
C2S C 0.6357(6) 0.0995(8) 0.0339(7) 0.045(2) Uani 1 1 d . . .
C3S C 0.7067(7) 0.1039(9) 0.1496(7) 0.059(3) Uani 1 1 d . . .
H3S1 H 0.6793 0.0234 0.1486 0.089 Uiso 1 1 calc R . .
H3S2 H 0.6941 0.1708 0.2199 0.089 Uiso 1 1 calc R . .
H3S3 H 0.7928 0.1204 0.1556 0.089 Uiso 1 1 calc R . .
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'
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 '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
N4 Pd1 P7 84.51(17) . . ?
N4 Pd1 P1 84.27(17) . . ?
P7 Pd1 P1 168.76(6) . . ?
N4 Pd1 Br1 177.39(14) . . ?
P7 Pd1 Br1 94.87(5) . . ?
P1 Pd1 Br1 96.37(5) . . ?
C21 P1 C11 105.5(3) . . ?
C21 P1 C2 106.2(3) . . ?
C11 P1 C2 107.7(3) . . ?
C21 P1 Pd1 119.1(2) . . ?
C11 P1 Pd1 116.9(2) . . ?
C2 P1 Pd1 100.3(3) . . ?
C16 C11 C12 120.2(6) . . ?
C16 C11 P1 120.2(5) . . ?
C12 C11 P1 119.6(5) . . ?
C11 C12 C13 118.9(7) . . ?
C14 C13 C12 120.6(7) . . ?
C13 C14 C15 120.5(7) . . ?
C14 C15 C16 119.9(7) . . ?
C11 C16 C15 119.8(6) . . ?
C22 C21 C26 119.0(7) . . ?
C22 C21 P1 120.6(5) . . ?
C26 C21 P1 120.2(6) . . ?
C23 C22 C21 121.0(6) . . ?
C22 C23 C24 119.3(7) . . ?
C25 C24 C23 119.7(7) . . ?
C26 C25 C24 120.8(7) . . ?
C25 C26 C21 120.0(7) . . ?
C3 C2 P1 108.3(5) . . ?
N4 C3 C2 109.1(5) . . ?
C5 N4 C3 113.1(5) . . ?
C5 N4 Pd1 113.7(4) . . ?
C3 N4 Pd1 112.9(4) . . ?
N4 C5 C6 108.6(5) . . ?
C5 C6 P7 107.3(4) . . ?
C41 P7 C31 108.5(3) . . ?
C41 P7 C6 105.4(3) . . ?
C31 P7 C6 106.0(3) . . ?
C41 P7 Pd1 118.5(2) . . ?
C31 P7 Pd1 116.9(2) . . ?
C6 P7 Pd1 99.7(2) . . ?
C32 C31 C36 119.5(6) . . ?
C32 C31 P7 120.9(5) . . ?
C36 C31 P7 119.5(5) . . ?
C33 C32 C31 120.8(7) . . ?
C32 C33 C34 119.9(7) . . ?
C35 C34 C33 119.5(7) . . ?
C34 C35 C36 121.1(7) . . ?
C35 C36 C31 119.1(7) . . ?
C42 C41 C46 118.9(6) . . ?
C42 C41 P7 118.9(5) . . ?
C46 C41 P7 122.2(5) . . ?
C43 C42 C41 120.0(6) . . ?
C42 C43 C44 121.5(7) . . ?
C43 C44 C45 120.0(6) . . ?
C44 C45 C46 119.7(7) . . ?
C45 C46 C41 119.9(6) . . ?
O1S C2S C1S 121.9(8) . . ?
O1S C2S C3S 120.1(8) . . ?
C1S C2S C3S 118.0(7) . . ?
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 N4 2.070(5) . ?
Pd1 P7 2.2991(19) . ?
Pd1 P1 2.3008(19) . ?
Pd1 Br1 2.4179(11) . ?
P1 C21 1.807(7) . ?
P1 C11 1.819(7) . ?
P1 C2 1.828(7) . ?
C11 C16 1.386(9) . ?
C11 C12 1.396(9) . ?
C12 C13 1.406(10) . ?
C13 C14 1.366(11) . ?
C14 C15 1.381(9) . ?
C15 C16 1.398(9) . ?
C21 C22 1.392(10) . ?
C21 C26 1.394(9) . ?
C22 C23 1.388(10) . ?
C23 C24 1.394(10) . ?
C24 C25 1.386(10) . ?
C25 C26 1.381(10) . ?
C2 C3 1.502(11) . ?
C3 N4 1.491(8) . ?
N4 C5 1.474(9) . ?
C5 C6 1.524(9) . ?
C6 P7 1.834(6) . ?
P7 C41 1.807(6) . ?
P7 C31 1.807(7) . ?
C31 C32 1.385(9) . ?
C31 C36 1.405(9) . ?
C32 C33 1.369(10) . ?
C33 C34 1.407(11) . ?
C34 C35 1.368(10) . ?
C35 C36 1.389(9) . ?
C41 C42 1.393(9) . ?
C41 C46 1.415(9) . ?
C42 C43 1.374(9) . ?
C43 C44 1.375(9) . ?
C44 C45 1.386(10) . ?
C45 C46 1.394(10) . ?
C1S C2S 1.491(12) . ?
O1S C2S 1.216(8) . ?
C2S C3S 1.503(10) . ?
