#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/83/2008343.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_2008343
loop_
_publ_author_name
'Rath, Nigam P. '
'Stockland Jr, Robert A.'
'Anderson, Gordon K.'
_publ_section_title
;
 [Bis(diphenylphosphino)methane]dinitratopalladium(II)
 tris(deuteriochloroform) solvate
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              494
_journal_page_last               496
_journal_paper_doi               10.1107/S0108270198016345
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '[Pd (N O3)2 (C25 H22 P2)], 3C D Cl3'
_chemical_formula_moiety         'C25 H22  N2 O6 P2 Pd .3(Cl D1 Cl3)'
_chemical_formula_sum            'C28 H22 Cl9 D3 N2 O6 P2 Pd'
_chemical_formula_weight         975.80
_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'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.
_cell_angle_beta                 93.8580(10)
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   13.9841(2)
_cell_length_b                   16.8118(2)
_cell_length_c                   16.8033(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     3941.47(9)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXTL-Plus
_computing_structure_refinement  SHELXTL-Plus
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1998)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.04
_diffrn_reflns_av_sigmaI/netI    0.0141
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            109227
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.203
_exptl_absorpt_correction_T_max  0.62
_exptl_absorpt_correction_T_min  0.54
_exptl_absorpt_correction_type   'empirical (SADABS; Blessing, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.353
_refine_diff_density_min         -1.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         9037
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.047
_refine_ls_R_factor_gt           0.040
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0478P)²+7.3285P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.109
_reflns_number_gt                7938
_reflns_number_total             9037
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fg1483.cif
_cod_data_source_block           fg1483
_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      'P 21/c'
_cod_original_formula_sum        'C28 H22 D3 Cl9 N2 O6 P2 Pd'
_cod_database_code               2008343
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_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 0.433882(15) 0.510369(12) 0.696876(12) 0.02900(7) Uani d . 1 . . Pd
P1 0.33914(5) 0.40781(4) 0.66325(4) 0.03195(15) Uani d . 1 . . P
P2 0.50455(5) 0.40086(4) 0.74813(4) 0.03147(15) Uani d . 1 . . P
O1 0.34452(15) 0.60166(13) 0.64480(13) 0.0403(5) Uani d . 1 . . O
O2 0.43965(18) 0.59291(16) 0.54807(15) 0.0508(6) Uani d . 1 . . O
O3 0.3242(2) 0.67883(18) 0.54230(17) 0.0622(7) Uani d . 1 . . O
O4 0.52940(15) 0.60319(12) 0.72952(13) 0.0387(5) Uani d . 1 . . O
O5 0.60351(18) 0.53837(14) 0.82786(14) 0.0468(5) Uani d . 1 . . O
O6 0.65176(19) 0.65381(15) 0.79483(19) 0.0596(7) Uani d . 1 . . O
N1 0.37042(18) 0.62469(16) 0.57583(16) 0.0392(6) Uani d . 1 . . N
N2 0.59649(18) 0.59757(15) 0.78589(15) 0.0351(5) Uani d . 1 . . N
C1 0.4323(2) 0.33253(18) 0.68292(19) 0.0377(6) Uani d . 1 . . C
H1A 0.4641 0.3167 0.6351 0.045 Uiso calc R 1 . . H
H1B 0.4099 0.2857 0.7109 0.045 Uiso calc R 1 . . H
C2 0.2907(2) 0.39998(18) 0.56175(18) 0.0351(6) Uani d . 1 . . C
C3 0.1986(3) 0.3740(4) 0.5432(3) 0.0817(17) Uani d . 1 . . C
H3 0.1577 0.3619 0.5836 0.098 Uiso calc R 1 . . H
C4 0.1672(4) 0.3659(5) 0.4631(3) 0.115(3) Uani d . 1 . . C
H4 0.1046 0.3478 0.4498 0.138 Uiso calc R 1 . . H
C5 0.2249(4) 0.3837(3) 0.4041(3) 0.0786(14) Uani d . 1 . . C
H5 0.2026 0.3773 0.3505 0.094 Uiso calc R 1 . . H
C6 0.3147(3) 0.4106(3) 0.4226(2) 0.0601(10) Uani d . 1 . . C
H6 0.3549 0.4230 0.3817 0.072 Uiso calc R 1 . . H
C7 0.3477(3) 0.4201(2) 0.50133(19) 0.0463(8) Uani d . 1 . . C
H7 0.4095 0.4404 0.5137 0.056 Uiso calc R 1 . . H
C8 0.2445(2) 0.39288(19) 0.72875(18) 0.0379(6) Uani d . 1 . . C
C9 0.2192(4) 0.3199(3) 0.7544(4) 0.096(2) Uani d . 1 . . C
H9 0.2534 0.2747 0.7397 0.115 Uiso calc R 1 . . H
C10 0.1427(5) 0.3120(3) 0.8025(5) 0.121(3) Uani d . 1 . . C
H10 0.1246 0.2610 0.8189 0.146 Uiso calc R 1 . . H
C11 0.0941(4) 0.3758(3) 0.8258(3) 0.0759(14) Uani d . 1 . . C
H11 0.0427 0.3695 0.8585 0.091 Uiso calc R 1 . . H
C12 0.1193(4) 0.4489(3) 0.8021(4) 0.0869(17) Uani d . 1 . . C
H12 0.0853 0.4937 0.8181 0.104 Uiso calc R 1 . . H
C13 0.1953(3) 0.4583(3) 0.7542(3) 0.0705(13) Uani d . 1 . . C
H13 0.2136 0.5096 0.7389 0.085 Uiso calc R 1 . . H
C14 0.6296(2) 0.38456(18) 0.73369(18) 0.0367(6) Uani d . 1 . . C
C15 0.6613(3) 0.3944(2) 0.6578(2) 0.0511(8) Uani d . 1 . . C
H15 0.6175 0.4081 0.6151 0.061 Uiso calc R 1 . . H
C16 0.7572(3) 0.3842(3) 0.6451(3) 0.0662(11) Uani d . 1 . . C
H16 0.7787 0.3911 0.5938 0.079 Uiso calc R 1 . . H
C17 0.8209(3) 0.3638(3) 0.7077(3) 0.0720(12) Uani d . 1 . . C
H17 0.8861 0.3571 0.6991 0.086 Uiso calc R 1 . . H
C18 0.7897(3) 0.3532(3) 0.7823(3) 0.0768(14) Uani d . 1 . . C
H18 0.8335 0.3387 0.8247 0.092 Uiso calc R 1 . . H
C19 0.6941(3) 0.3636(3) 0.7958(2) 0.0582(10) Uani d . 1 . . C
H19 0.6730 0.3563 0.8473 0.070 Uiso calc R 1 . . H
C20 0.4761(2) 0.37520(17) 0.84784(17) 0.0349(6) Uani d . 1 . . C
C21 0.4816(3) 0.2961(2) 0.8721(2) 0.0489(8) Uani d . 1 . . C
H21 0.5043 0.2571 0.8380 0.059 Uiso calc R 1 . . H
C22 0.4536(3) 0.2751(2) 0.9464(2) 0.0605(10) Uani d . 1 . . C
H22 0.4579 0.2218 0.9631 0.073 Uiso calc R 1 . . H
C23 0.4192(3) 0.3321(2) 0.9965(2) 0.0569(9) Uani d . 1 . . C
H23 0.4001 0.3175 1.0470 0.068 Uiso calc R 1 . . H
C24 0.4129(3) 0.4103(2) 0.9725(2) 0.0524(9) Uani d . 1 . . C
H24 0.3893 0.4489 1.0066 0.063 Uiso calc R 1 . . H
C25 0.4414(2) 0.43224(19) 0.89817(19) 0.0409(7) Uani d . 1 . . C
H25 0.4371 0.4857 0.8819 0.049 Uiso calc R 1 . . H
C1S 0.1192(3) 0.6549(3) 0.5983(3) 0.0689(12) Uani d . 1 . . C
H1S 0.1875 0.6623 0.6164 0.083 Uiso d R 1 A . H
Cl1 0.08537(11) 0.73371(9) 0.53545(9) 0.0898(4) Uani d . 1 A 1 Cl
Cl2 0.05291(10) 0.65486(11) 0.68190(8) 0.0919(4) Uani d . 1 A 1 Cl
Cl3 0.1113(3) 0.56453(14) 0.55002(19) 0.0862(10) Uani d P 0.822(14) A 1 Cl
Cl3' 0.071(2) 0.5744(19) 0.524(2) 0.203(12) Uani d P 0.178(14) A 2 Cl
C2S 0.2847(4) 0.6773(3) 0.9096(3) 0.0668(11) Uani d . 1 . . C
H2S 0.2890 0.7323 0.9307 0.080 Uiso calc R 1 . . H
Cl4 0.31900(13) 0.61193(10) 0.98594(8) 0.0938(4) Uani d . 1 . . Cl
Cl5 0.36159(16) 0.66824(9) 0.83267(10) 0.1167(7) Uani d . 1 . . Cl
Cl6 0.16554(14) 0.65799(12) 0.87609(13) 0.1280(7) Uani d . 1 . . Cl
C3S 0.1583(3) 0.0875(2) 0.60672(19) 0.0795(15) Uani d D 1 . . C
H3S 0.2272 0.0765 0.6191 0.095 Uiso d R 1 B . H
Cl7 0.1083(2) 0.0839(3) 0.69458(14) 0.1264(14) Uani d PD 0.717(4) B 1 Cl
Cl8 0.1542(3) 0.17419(19) 0.55659(19) 0.1419(14) Uani d PD 0.717(4) B 1 Cl
Cl9 0.1161(3) 0.00850(18) 0.54597(16) 0.1401(14) Uani d PD 0.717(4) B 1 Cl
Cl7' 0.1315(9) 0.0211(8) 0.6755(9) 0.222(8) Uani d PD 0.283(4) B 2 Cl
Cl8' 0.1450(8) 0.1051(8) 0.5087(3) 0.176(5) Uani d PD 0.283(4) B 2 Cl
Cl9' 0.0887(6) 0.1687(4) 0.6353(7) 0.170(5) Uani d PD 0.283(4) B 2 Cl
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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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_publ_flag
O4 Pd1 O1 85.26(9) ?
O4 Pd1 P1 177.04(6) ?
O1 Pd1 P1 97.54(7) yes
O4 Pd1 P2 104.72(6) yes
O1 Pd1 P2 169.78(7) ?
P1 Pd1 P2 72.52(3) yes
C8 P1 C2 108.96(14) ?
C8 P1 C1 109.75(15) ?
C2 P1 C1 109.82(14) ?
C8 P1 Pd1 113.82(11) ?
C2 P1 Pd1 118.57(10) ?
C1 P1 Pd1 94.91(10) ?
C8 P1 P2 108.56(11) ?
C2 P1 P2 140.46(10) ?
C1 P1 P2 44.27(9) ?
Pd1 P1 P2 53.92(2) ?
C20 P2 C14 111.48(14) ?
C20 P2 C1 104.91(15) ?
C14 P2 C1 108.87(14) ?
C20 P2 Pd1 115.86(10) ?
C14 P2 Pd1 118.77(11) ?
C1 P2 Pd1 94.24(10) ?
C20 P2 P1 105.84(10) ?
C14 P2 P1 139.25(10) ?
C1 P2 P1 43.93(10) ?
Pd1 P2 P1 53.56(2) ?
N1 O1 Pd1 113.01(18) ?
N2 O4 Pd1 123.69(17) ?
O2 N1 O3 123.5(3) ?
O2 N1 O1 119.1(2) ?
O3 N1 O1 117.4(3) ?
O5 N2 O6 122.3(3) ?
O5 N2 O4 120.7(2) ?
O6 N2 O4 117.1(3) ?
P1 C1 P2 91.80(14) ?
C7 C2 C3 119.4(3) ?
C7 C2 P1 118.8(2) ?
C3 C2 P1 121.8(3) ?
C2 C3 C4 118.7(4) ?
C5 C4 C3 121.4(4) ?
C6 C5 C4 119.8(4) ?
C5 C6 C7 120.3(4) ?
C2 C7 C6 120.4(3) ?
C9 C8 C13 118.5(3) ?
C9 C8 P1 122.7(3) ?
C13 C8 P1 118.8(3) ?
C8 C9 C10 120.0(4) ?
C11 C10 C9 121.1(4) ?
C10 C11 C12 119.7(4) ?
C11 C12 C13 120.2(4) ?
C8 C13 C12 120.5(4) ?
C19 C14 C15 119.6(3) ?
C19 C14 P2 121.9(3) ?
C15 C14 P2 118.5(2) ?
C16 C15 C14 120.0(3) ?
C17 C16 C15 119.9(4) ?
C18 C17 C16 120.3(4) ?
C17 C18 C19 120.4(4) ?
C14 C19 C18 119.9(4) ?
C25 C20 C21 119.8(3) ?
C25 C20 P2 120.7(2) ?
C21 C20 P2 119.4(2) ?
C22 C21 C20 119.7(3) ?
C21 C22 C23 120.3(3) ?
C24 C23 C22 120.1(3) ?
C23 C24 C25 120.1(3) ?
C24 C25 C20 119.9(3) ?
Cl3 C1S Cl2 111.1(3) ?
Cl3 C1S Cl1 112.3(3) ?
Cl2 C1S Cl1 110.7(3) ?
Cl3 C1S Cl3' 21.4(13) ?
Cl2 C1S Cl3' 110.1(7) ?
Cl1 C1S Cl3' 94.1(15) ?
Cl4 C2S Cl5 109.9(3) ?
Cl4 C2S Cl6 109.3(3) ?
Cl5 C2S Cl6 111.4(3) ?
Cl7' C3S Cl8' 141.8(9) ?
Cl7' C3S Cl7 40.5(5) ?
Cl8' C3S Cl7 148.1(5) ?
Cl7' C3S Cl8 157.7(6) ?
Cl8' C3S Cl8 49.8(5) ?
Cl7 C3S Cl8 118.0(3) ?
Cl7' C3S Cl9 79.2(7) ?
Cl8' C3S Cl9 63.2(5) ?
Cl7 C3S Cl9 110.0(3) ?
Cl8 C3S Cl9 111.5(2) ?
Cl7' C3S Cl9' 100.1(6) ?
Cl8' C3S Cl9' 96.0(6) ?
Cl7 C3S Cl9' 61.1(4) ?
Cl8 C3S Cl9' 57.6(4) ?
Cl9 C3S Cl9' 125.1(4) ?
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 O4 . 2.103(2) yes
Pd1 O1 . 2.130(2) yes
Pd1 P1 . 2.2241(8) yes
Pd1 P2 . 2.2345(7) yes
P1 C8 . 1.795(3) ?
P1 C2 . 1.797(3) ?
P1 C1 . 1.831(3) ?
P1 P2 . 2.6371(11) ?
P2 C20 . 1.801(3) ?
P2 C14 . 1.803(3) ?
P2 C1 . 1.842(3) ?
O1 N1 . 1.296(3) ?
O2 N1 . 1.225(4) ?
O3 N1 . 1.231(4) ?
O4 N2 . 1.291(3) ?
O5 N2 . 1.220(3) ?
O6 N2 . 1.224(3) ?
C2 C7 . 1.375(4) ?
C2 C3 . 1.375(5) ?
C3 C4 . 1.393(6) ?
C4 C5 . 1.353(7) ?
C5 C6 . 1.352(6) ?
C6 C7 . 1.380(5) ?
C8 C9 . 1.355(5) ?
C8 C13 . 1.379(5) ?
C9 C10 . 1.390(6) ?
C10 C11 . 1.343(7) ?
C11 C12 . 1.346(7) ?
C12 C13 . 1.384(6) ?
C14 C19 . 1.378(5) ?
C14 C15 . 1.388(5) ?
C15 C16 . 1.383(5) ?
C16 C17 . 1.375(6) ?
C17 C18 . 1.367(7) ?
C18 C19 . 1.383(6) ?
C20 C25 . 1.388(4) ?
C20 C21 . 1.391(4) ?
C21 C22 . 1.380(5) ?
C22 C23 . 1.383(6) ?
C23 C24 . 1.375(5) ?
C24 C25 . 1.386(5) ?
C1S Cl3 . 1.722(6) ?
C1S Cl2 . 1.735(5) ?
C1S Cl1 . 1.740(5) ?
C1S Cl3' . 1.932(19) ?
C2S Cl4 . 1.731(5) ?
C2S Cl5 . 1.743(5) ?
C2S Cl6 . 1.753(5) ?
C3S Cl7' . 1.668(5) ?
C3S Cl8' . 1.671(5) ?
C3S Cl7 . 1.676(3) ?
C3S Cl8 . 1.682(4) ?
C3S Cl9 . 1.753(4) ?
C3S Cl9' . 1.761(5) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C1 H1B O6 2_646 0.98 2.38 3.257(4) 149 yes
C1S H1S O1 . 0.99 2.44 3.318(5) 148 yes
C1S H1S O3 . 0.99 2.37 3.103(5) 131 yes
C2S H2S O3 4_576 0.99 2.42 3.310(6) 149 yes
C3S H3S O6 2_646 0.99 2.51 3.232(5) 129 yes
C6 H6 O4 3_666 0.94 2.59 3.477(4) 157 yes
C7 H7 O2 3_666 0.94 2.48 3.148(5) 128 yes
C9 H9 O6 2_646 0.94 2.52 3.455(6) 178 yes
