#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/06/2010668.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2010668
loop_
_publ_author_name
'Abu-Surrah, Adnan S.'
'Debaerdemaeker, Tony'
'Huhn, Wolfgang'
'Rieger, Bernhard'
'Klinga, Martti'
'Repo, Timo'
'Leskelä, Markku'
_publ_section_title
;
 An alkyl--palladium(II) complex with a bidentate phosphine ligand:
 [1,3-bis(diphenylphosphino)propane-P,P']dimethylpalladium(II)
 toluene hemisolvate
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              e42
_journal_page_last               e43
_journal_paper_doi               10.1107/S0108270100000391
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[Pd (C H3)2 (C27 H26 P2)], 0.5C7 H8'
_chemical_formula_sum            'C32.5 H36 P2 Pd'
_chemical_formula_weight         594.95
_chemical_name_systematic
;
Dimethyl[1,3-bis(diphenylphosphino)propane]palladium(II) hemitoluene
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELX97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.00(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.260(3)
_cell_length_b                   15.025(2)
_cell_length_c                   16.347(3)
_cell_measurement_reflns_used    4521
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.10
_cell_measurement_theta_min      2.16
_cell_volume                     2974.2(10)
_computing_cell_refinement       IDPS
_computing_data_collection       'IDPS (Stoe & Cie, 1997))'
_computing_data_reduction        IDPS
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'XMY93 (Debaermaeker, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean .15
_diffrn_measured_fraction_theta_full .917
_diffrn_measured_fraction_theta_max .917
_diffrn_measurement_device_type  'Stoe-IPDS image-plate'
_diffrn_measurement_method       rotation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .034
_diffrn_reflns_av_sigmaI/netI    .0213
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22466
_diffrn_reflns_theta_full        24.10
_diffrn_reflns_theta_max         24.10
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        <2
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    .750
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          .45
_exptl_crystal_size_mid          .40
_exptl_crystal_size_min          .35
_refine_diff_density_max         .28
_refine_diff_density_min         -.20
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         4521
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          .030
_refine_ls_R_factor_gt           .023
_refine_ls_shift/su_max          .002
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0393P)²+0.2200P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .062
_reflns_number_gt                3825
_reflns_number_total             4521
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            qb0151.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0393P)^2^+0.2200P] where P = (Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0393P)^2^+0.2200P] where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C32.50 H36 P2 Pd'
_cod_database_code               2010668
_cod_database_fobs_code          2010668
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Pd1 .112737(13) .626486(12) .218962(9) .04119(7) Uani d . 1 . . Pd
P1 .04181(5) .56046(5) .32618(3) .04852(16) Uani d . 1 . . P
P2 .24781(5) .51983(4) .21929(3) .04253(14) Uani d . 1 . . P
C1 .1380(2) .4962(2) .40105(14) .0627(7) Uani d . 1 . . C
H1A .1919 .5375 .4326 .075 Uiso calc R 1 . . H
H1B .0961 .4673 .4409 .075 Uiso calc R 1 . . H
C2 .2003(2) .42523(19) .36082(14) .0582(7) Uani d . 1 . . C
H2A .1470 .3920 .3203 .070 Uiso calc R 1 . . H
H2B .2330 .3826 .4040 .070 Uiso calc R 1 . . H
C3 .29190(19) .46105(18) .31673(14) .0524(6) Uani d . 1 . . C
H3A .3392 .4105 .3056 .063 Uiso calc R 1 . . H
H3B .3382 .5020 .3550 .063 Uiso calc R 1 . . H
C4 .38276(19) .5544(2) .19665(15) .0575(7) Uani d . 1 . . C
C5 .4223(3) .6360(2) .22433(19) .0802(9) Uani d . 1 . . C
H5 .3768 .6747 .2502 .096 Uiso calc R 1 . . H
C6 .5282(3) .6629(4) .2151(3) .1131(15) Uani d U 1 . . C
H6 .5549 .7195 .2352 .136 Uiso calc R 1 . . H
C7 .5926(3) .6092(5) .1780(3) .1263(19) Uani d U 1 . . C
H7 .6650 .6277 .1717 .152 Uiso calc R 1 . . H
C8 .5551(3) .5289(4) .1493(3) .1313(18) Uani d U 1 . . C
H8 .6011 .4914 .1227 .158 Uiso calc R 1 . . H
C9 .4490(3) .5002(3) .1585(2) .0919(11) Uani d . 1 . . C
H9 .4232 .4434 .1384 .110 Uiso calc R 1 . . H
C10 .2057(2) .43200(18) .14431(14) .0510(6) Uani d . 1 . . C
C11 .2171(3) .3432(2) .16084(18) .0748(8) Uani d . 1 . . C
H11 .2500 .3243 .2145 .090 Uiso calc R 1 . . H
C12 .1812(4) .2797(3) .1003(2) .0979(11) Uani d . 1 . . C
H12 .1878 .2181 .1133 .117 Uiso calc R 1 . . H
C13 .1377(4) .3056(3) .0240(2) .1121(14) Uani d U 1 . . C
H13 .1158 .2623 -.0177 .135 Uiso calc R 1 . . H
C14 .1246(5) .3925(3) .0059(2) .1315(18) Uani d U 1 . . C
H14 .0934 .4105 -.0485 .158 Uiso calc R 1 . . H
C15 .1567(3) .4562(2) .06664(18) .0946(12) Uani d U 1 . . C
H15 .1445 .5174 .0539 .113 Uiso calc R 1 . . H
C16 -.0167(2) .63715(19) .39387(15) .0617(7) Uani d . 1 . . C
C17 -.1268(3) .6459(2) .3978(2) .0794(9) Uani d . 1 . . C
H17 -.1791 .6080 .3659 .095 Uiso calc R 1 . . H
C18 -.1622(4) .7116(3) .4495(3) .0995(12) Uani d . 1 . . C
H18 -.2384 .7169 .4534 .119 Uiso calc R 1 . . H
C19 -.0891(5) .7665(3) .4932(2) .1083(14) Uani d . 1 . . C
H19 -.1140 .8108 .5273 .130 Uiso calc R 1 . . H
C20 .0181(5) .7596(3) .4891(3) .1299(17) Uani d . 1 . . C
H20 .0694 .7992 .5198 .156 Uiso calc R 1 . . H
C21 .0542(3) .6949(3) .4403(2) .1053(13) Uani d . 1 . . C
H21 .1311 .6900 .4387 .126 Uiso calc R 1 . . H
C22 -.0661(2) .47956(18) .29188(16) .0570(6) Uani d . 1 . . C
C23 -.0948(2) .4642(2) .20833(18) .0760(9) Uani d . 1 . . C
H23 -.0593 .4967 .1702 .091 Uiso calc R 1 . . H
C24 -.1752(3) .4015(3) .1787(3) .0984(11) Uani d . 1 . . C
H24 -.1939 .3913 .1209 .118 Uiso calc R 1 . . H
C25 -.2265(3) .3553(3) .2329(3) .1001(12) Uani d . 1 . . C
H25 -.2825 .3135 .2129 .120 Uiso calc R 1 . . H
C26 -.1985(3) .3682(2) .3149(3) .0963(12) Uani d . 1 . . C
H26 -.2343 .3347 .3523 .116 Uiso calc R 1 . . H
C27 -.1184(3) .4293(2) .3456(2) .0806(9) Uani d . 1 . . C
H27 -.0990 .4371 .4037 .097 Uiso calc R 1 . . H
C28 .1634(2) .69323(19) .11963(15) .0620(7) Uani d . 1 . . C
H28A .2316 .6663 .1070 .074 Uiso calc R 1 . . H
H28B .1767 .7560 .1341 .074 Uiso calc R 1 . . H
H28C .1057 .6888 .0710 .074 Uiso calc R 1 . . H
C29 -.0101(3) .7237(2) .21083(17) .0710(8) Uani d . 1 . . C
H29A -.0825 .6950 .2074 .085 Uiso calc R 1 . . H
H29B -.0085 .7599 .1612 .085 Uiso calc R 1 . . H
H29C .0029 .7618 .2601 .085 Uiso calc R 1 . . H
C31 -.0360(5) .0013(6) .0321(3) .088(2) Uani d PD .50 A 1 C
C32 .0007(9) .0733(6) -.0073(6) .073(4) Uani d PD .50 A 1 C
H32A -.0164 .1326 .0085 .088 Uiso d PR .50 A 1 H
C33 .0666(6) .0620(5) -.0673(5) .097(2) Uani d PD .50 A 1 C
H33A .0907 .1117 -.0968 .116 Uiso d PR .50 A 1 H
C34 .1002(14) -.0228(7) -.0852(10) .136(7) Uani d PD .50 A 1 C
H34A .1499 -.0330 -.1241 .163 Uiso d PR .50 A 1 H
C35 .0558(7) -.0957(5) -.0509(7) .119(3) Uani d PD .50 A 1 C
H35A .0687 -.1554 -.0680 .143 Uiso d PR .50 A 1 H
C36 -.0100(14) -.0839(7) .0093(10) .122(9) Uani d PD .50 A 1 C
H36A -.0334 -.1332 .0396 .146 Uiso d PR .50 A 1 H
C37 -.0959(12) .0141(9) .1035(8) .133(8) Uani d PD .50 A 1 C
H37A -.1123 -.0457 .1181 .159 Uiso d PR .50 A 1 H
H37B -.0537 .0431 .1504 .159 Uiso d PR .50 A 1 H
H37C -.1635 .0461 .0869 .159 Uiso d PR .50 A 1 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -.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_publ_flag
C28 Pd1 C29 85.05(11) y
C28 Pd1 P1 174.63(8) y
C29 Pd1 P1 89.72(8) y
C28 Pd1 P2 92.00(8) y
C29 Pd1 P2 176.49(7) y
P1 Pd1 P2 93.19(3) y
C22 P1 C16 105.84(13) ?
C22 P1 C1 102.38(14) ?
C16 P1 C1 101.59(12) ?
C22 P1 Pd1 113.38(8) ?
C16 P1 Pd1 114.97(9) ?
C1 P1 Pd1 117.07(9) ?
C10 P2 C4 103.91(12) ?
C10 P2 C3 104.52(12) ?
C4 P2 C3 99.22(11) ?
C10 P2 Pd1 112.01(8) ?
C4 P2 Pd1 118.38(10) ?
C3 P2 Pd1 116.91(8) ?
C2 C1 P1 113.24(16) ?
C1 C2 C3 114.5(2) ?
C2 C3 P2 116.32(16) ?
C9 C4 C5 118.7(3) ?
C9 C4 P2 122.9(3) ?
C5 C4 P2 118.2(2) ?
C4 C5 C6 120.9(4) ?
C7 C6 C5 120.0(5) ?
C6 C7 C8 120.2(4) ?
C7 C8 C9 120.7(5) ?
C4 C9 C8 119.5(4) ?
C11 C10 C15 117.4(3) ?
C11 C10 P2 124.49(19) ?
C15 C10 P2 118.1(2) ?
C10 C11 C12 121.1(3) ?
C13 C12 C11 119.9(4) ?
C12 C13 C14 120.4(3) ?
C13 C14 C15 120.0(3) ?
C10 C15 C14 121.0(3) ?
C17 C16 C21 117.3(3) ?
C17 C16 P1 125.1(3) ?
C21 C16 P1 117.4(2) ?
C16 C17 C18 119.6(4) ?
C19 C18 C17 120.5(4) ?
C20 C19 C18 120.6(4) ?
C19 C20 C21 119.6(5) ?
C16 C21 C20 122.4(4) ?
C23 C22 C27 117.7(3) ?
C23 C22 P1 118.6(2) ?
C27 C22 P1 123.6(2) ?
C22 C23 C24 121.0(3) ?
C25 C24 C23 119.6(4) ?
C26 C25 C24 120.3(4) ?
C25 C26 C27 121.0(3) ?
C26 C27 C22 120.3(3) ?
C32 C31 C36 119.8(6) ?
C32 C31 C37 120.4(7) ?
C36 C31 C37 119.7(7) ?
C31 C32 C33 120.7(6) ?
C32 C33 C34 119.4(7) ?
C35 C34 C33 119.7(7) ?
C36 C35 C34 120.0(7) ?
C35 C36 C31 119.7(7) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 C28 . 2.084(2) y
Pd1 C29 . 2.087(3) y
Pd1 P1 . 2.2999(7) y
Pd1 P2 . 2.3038(7) y
P1 C22 . 1.820(3) ?
P1 C16 . 1.821(3) ?
P1 C1 . 1.835(2) ?
P2 C10 . 1.820(3) ?
P2 C4 . 1.827(2) ?
P2 C3 . 1.828(2) ?
C1 C2 . 1.520(4) ?
C2 C3 . 1.524(3) ?
C4 C9 . 1.368(4) ?
C4 C5 . 1.368(4) ?
C5 C6 . 1.390(5) ?
C6 C7 . 1.340(7) ?
C7 C8 . 1.348(7) ?
C8 C9 . 1.401(5) ?
C10 C11 . 1.364(4) ?
C10 C15 . 1.366(4) ?
C11 C12 . 1.395(5) ?
C12 C13 . 1.335(5) ?
C13 C14 . 1.344(6) ?
C14 C15 . 1.390(5) ?
C16 C17 . 1.367(4) ?
C16 C21 . 1.371(5) ?
C17 C18 . 1.411(5) ?
C18 C19 . 1.339(6) ?
C19 C20 . 1.330(7) ?
C20 C21 . 1.374(5) ?
C22 C23 . 1.376(4) ?
C22 C27 . 1.388(4) ?
C23 C24 . 1.393(5) ?
C24 C25 . 1.356(5) ?
C25 C26 . 1.344(6) ?
C26 C27 . 1.381(5) ?
C31 C32 . 1.371(7) ?
C31 C36 . 1.384(8) ?
C31 C37 . 1.486(7) ?
C32 C33 . 1.375(7) ?
C33 C34 . 1.385(8) ?
C34 C35 . 1.380(8) ?
C35 C36 . 1.378(8) ?
