#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2006204.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_2006204
loop_
_publ_author_name
'Sommerer, S. O.'
'Jircitano, A. J.'
'Westcott, B. L.'
'Abboud, K. A.'
'Krause Bauer, J. A.'
_publ_section_title
;
Bis(di-2-pyridylmethanediol-N,N')palladium(II)
Dichloride Tetrahydrate and
Dichloro(di-2-pyridylmethanediol-N,N')gold(III) Chloride
;
_journal_issue 6
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 707
_journal_page_last 710
_journal_volume 53
_journal_year 1997
_chemical_formula_moiety '[Pd(C11 H10 N2 O2)2]Cl2 , 4H2 O'
_chemical_formula_sum 'C22 H28 Cl2 N4 O8 Pd'
_chemical_formula_weight 653.78
_chemical_name_systematic
;
Bis(2,2'-dipyridylmethanediol-N,N')palladium(II) Chloride Tetrahydrate
;
_space_group_IT_number 15
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 1 2/c 1'
_audit_creation_method SHELXL
_cell_angle_alpha 90.00
_cell_angle_beta 91.080(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 14.814(3)
_cell_length_b 12.372(2)
_cell_length_c 14.306(2)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 22
_cell_measurement_theta_min 20
_cell_volume 2621.5(8)
_computing_cell_refinement SHELXTL-Plus
_computing_data_collection 'SHELXTL-Plus (Sheldrick, 1991)'
_computing_data_reduction SHELXTL-Plus
_computing_molecular_graphics 'ORTEX (McArdle, 1995)'
_computing_publication_material SHELXS86
_computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution 'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature 293(2)
_diffrn_measurement_device 'Nicolet P3'
_diffrn_measurement_method \q-2\q
_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 0.0000
_diffrn_reflns_av_sigmaI/netI 0.0162
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 3041
_diffrn_reflns_theta_max 27.56
_diffrn_reflns_theta_min 2.14
_diffrn_standards_decay_% 1
_diffrn_standards_interval_count 300
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.965
_exptl_absorpt_correction_T_max 0.277
_exptl_absorpt_correction_T_min 0.230
_exptl_absorpt_correction_type analytical
_exptl_crystal_colour Light-yellow
_exptl_crystal_density_diffrn 1.656
_exptl_crystal_density_meas 'not measured'
_exptl_crystal_description rod
_exptl_crystal_F_000 1328
_exptl_crystal_size_max 0.55
_exptl_crystal_size_mid 0.40
_exptl_crystal_size_min 0.25
_refine_diff_density_max 1.032
_refine_diff_density_min -0.814
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_all 1.054
_refine_ls_goodness_of_fit_obs 1.098
_refine_ls_matrix_type full
_refine_ls_number_parameters 171
_refine_ls_number_reflns 3041
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.054
_refine_ls_restrained_S_obs 1.098
_refine_ls_R_factor_all 0.0429
_refine_ls_R_factor_obs 0.0364
_refine_ls_shift/esd_max 0.000
_refine_ls_shift/esd_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.0470P)^2^+4.5639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all 0.1206
_refine_ls_wR_factor_obs 0.1144
_reflns_number_observed 2545
_reflns_number_total 3041
_reflns_observed_criterion >2sigma(I)
_[local]_cod_data_source_file fg1220.cif
_[local]_cod_data_source_block I
_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_values 1715 2011-07-08 13:25:40Z adriana
;
_cod_database_code 2006204
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Pd 0.0234(2) 0.0255(2) 0.0284(2) 0.00016(10) 0.00570(12) -0.00135(11)
Cl1 0.0587(6) 0.0765(8) 0.0683(7) -0.0084(6) 0.0057(5) -0.0107(6)
O1 0.0326(11) 0.0434(13) 0.0293(10) 0.0035(10) -0.0011(8) 0.0011(9)
O2 0.0430(13) 0.0368(13) 0.0448(13) 0.0145(10) 0.0103(10) -0.0010(10)
N1 0.0273(12) 0.0277(12) 0.0306(11) -0.0010(9) 0.0022(9) 0.0002(10)
N2 0.0262(12) 0.0309(13) 0.0297(12) -0.0004(9) 0.0050(10) 0.0002(9)
C1 0.0279(14) 0.042(2) 0.038(2) -0.0033(13) 0.0023(12) 0.0029(13)
C2 0.037(2) 0.050(2) 0.041(2) -0.015(2) -0.0022(14) 0.0046(15)
C3 0.057(2) 0.035(2) 0.047(2) -0.016(2) -0.001(2) -0.0020(15)
C4 0.048(2) 0.031(2) 0.041(2) -0.0021(14) 0.0003(14) -0.0046(13)
C5 0.0334(15) 0.0285(14) 0.0270(13) 0.0012(12) 0.0029(11) 0.0003(11)
C6 0.0304(14) 0.0305(15) 0.0314(14) 0.0059(12) 0.0036(11) -0.0016(12)
C7 0.0244(13) 0.0341(15) 0.0281(13) -0.0008(11) 0.0020(10) -0.0030(11)
C8 0.033(2) 0.047(2) 0.033(2) 0.0016(14) 0.0081(12) -0.0025(14)
C9 0.046(2) 0.055(2) 0.031(2) -0.009(2) 0.0147(14) 0.000(2)
C10 0.051(2) 0.040(2) 0.039(2) -0.010(2) 0.0050(15) 0.0079(15)
C11 0.038(2) 0.032(2) 0.037(2) 0.0003(13) 0.0040(13) 0.0010(13)
OW1 0.066(2) 0.125(3) 0.066(2) -0.015(2) 0.015(2) -0.005(2)
OW2 0.0200(9) 0.067(2) 0.0288(10) -0.0057(10) 0.0060(8) 0.0011(10)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Pd 0.0000 0.0000 0.5000 0.02570(13) Uani d S 1 Pd
Cl1 0.37818(8) 0.10800(11) 0.63284(9) 0.0678(3) Uani d . 1 Cl
O1 0.1362(2) -0.1588(2) 0.50632(15) 0.0351(5) Uani d . 1 O
HO1 0.1879(11) -0.135(4) 0.5101(3) 0.053 Uiso calc R 1 H
O2 0.1673(2) -0.2539(2) 0.3715(2) 0.0414(6) Uani d . 1 O
HO2 0.166(3) -0.3096(14) 0.402(2) 0.062 Uiso calc R 1 H
N1 -0.0459(2) -0.1406(2) 0.4453(2) 0.0285(5) Uani d . 1 N
N2 0.0765(2) 0.0139(2) 0.3850(2) 0.0289(5) Uani d . 1 N
C1 -0.1351(2) -0.1635(3) 0.4415(2) 0.0358(7) Uani d . 1 C
H1 -0.1760(2) -0.1141(3) 0.4654(2) 0.043 Uiso calc R 1 H
C2 -0.1667(2) -0.2587(3) 0.4029(2) 0.0427(8) Uani d . 1 C
H2 -0.2283(2) -0.2732(3) 0.4004(2) 0.051 Uiso calc R 1 H
C3 -0.1063(3) -0.3317(3) 0.3682(3) 0.0460(9) Uani d . 1 C
H3 -0.1266(3) -0.3967(3) 0.3428(3) 0.055 Uiso calc R 1 H
C4 -0.0149(3) -0.3082(3) 0.3713(2) 0.0398(7) Uani d . 1 C
H4 0.0268(3) -0.3569(3) 0.3478(2) 0.048 Uiso calc R 1 H
C5 0.0134(2) -0.2109(2) 0.4099(2) 0.0296(6) Uani d . 1 C
C6 0.1127(2) -0.1768(2) 0.4122(2) 0.0308(6) Uani d . 1 C
C7 0.1236(2) -0.0730(3) 0.3555(2) 0.0289(6) Uani d . 1 C
C8 0.1802(2) -0.0656(3) 0.2791(2) 0.0377(7) Uani d . 1 C
H8 0.2131(2) -0.1253(3) 0.2599(2) 0.045 Uiso calc R 1 H
C9 0.1867(3) 0.0316(4) 0.2326(2) 0.0437(8) Uani d . 1 C
H9 0.2247(3) 0.0379(4) 0.1818(2) 0.052 Uiso calc R 1 H
C10 0.1371(3) 0.1193(3) 0.2611(2) 0.0431(8) Uani d . 1 C
H10 0.1402(3) 0.1848(3) 0.2293(2) 0.052 Uiso calc R 1 H
C11 0.0824(2) 0.1081(3) 0.3381(2) 0.0358(7) Uani d . 1 C
H11 0.0489(2) 0.1672(3) 0.3580(2) 0.043 Uiso calc R 1 H
OW1 0.4114(3) -0.1128(4) 0.3490(3) 0.0854(12) Uani d . 1 O
OW2 0.30970(14) -0.0640(2) 0.50665(15) 0.0386(6) Uani d . 1 O
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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Pd N1 5_556 . 180.0 ?
N1 Pd N2 5_556 5_556 87.02(10) ?
N1 Pd N2 . 5_556 92.98(10) yes
N1 Pd N2 5_556 . 92.98(10) ?
N1 Pd N2 . . 87.02(10) yes
N2 Pd N2 5_556 . 180.0 ?
C6 O1 HO1 . . 109.5(2) yes
C6 O2 HO2 . . 109.5(2) yes
C5 N1 C1 . . 119.7(3) yes
C5 N1 Pd . . 119.1(2) yes
C1 N1 Pd . . 121.2(2) yes
C11 N2 C7 . . 119.5(3) yes
C11 N2 Pd . . 121.4(2) yes
C7 N2 Pd . . 119.1(2) yes
N1 C1 C2 . . 121.3(3) yes
N1 C1 H1 . . 119.4(2) ?
C2 C1 H1 . . 119.4(2) ?
C3 C2 C1 . . 119.3(3) yes
C3 C2 H2 . . 120.4(2) ?
C1 C2 H2 . . 120.4(2) ?
C2 C3 C4 . . 119.6(3) yes
C2 C3 H3 . . 120.2(2) ?
C4 C3 H3 . . 120.2(2) ?
C5 C4 C3 . . 118.9(3) yes
C5 C4 H4 . . 120.6(2) ?
C3 C4 H4 . . 120.6(2) ?
N1 C5 C4 . . 121.2(3) yes
N1 C5 C6 . . 116.7(3) yes
C4 C5 C6 . . 122.1(3) yes
O2 C6 O1 . . 112.2(3) yes
O2 C6 C7 . . 106.7(2) yes
O1 C6 C7 . . 110.5(3) yes
O2 C6 C5 . . 111.7(3) yes
O1 C6 C5 . . 106.6(2) yes
C7 C6 C5 . . 109.3(2) yes
N2 C7 C8 . . 120.9(3) yes
N2 C7 C6 . . 116.2(2) yes
C8 C7 C6 . . 122.9(3) yes
C9 C8 C7 . . 119.1(3) yes
C9 C8 H8 . . 120.5(2) ?
C7 C8 H8 . . 120.5(2) ?
C10 C9 C8 . . 120.0(3) yes
C10 C9 H9 . . 120.0(2) ?
C8 C9 H9 . . 120.0(2) ?
C9 C10 C11 . . 118.7(3) yes
C9 C10 H10 . . 120.7(2) ?
C11 C10 H10 . . 120.7(2) ?
N2 C11 C10 . . 121.7(3) yes
N2 C11 H11 . . 119.1(2) ?
C10 C11 H11 . . 119.1(2) ?
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
Pd N1 5_556 2.020(3) ?
Pd N1 . 2.020(3) yes
Pd N2 5_556 2.022(3) ?
Pd N2 . 2.022(3) yes
O1 C6 . 1.401(4) yes
O1 HO1 . 0.82 ?
O2 C6 . 1.385(3) yes
O2 HO2 . 0.82 ?
N1 C5 . 1.342(4) yes
N1 C1 . 1.352(4) yes
N2 C11 . 1.348(4) yes
N2 C7 . 1.354(4) yes
C1 C2 . 1.379(5) yes
C1 H1 . 0.93 ?
C2 C3 . 1.371(6) yes
C2 H2 . 0.93 ?
C3 C4 . 1.385(5) yes
C3 H3 . 0.93 ?
C4 C5 . 1.387(4) yes
C4 H4 . 0.93 ?
C5 C6 . 1.530(4) yes
C6 C7 . 1.529(4) yes
C7 C8 . 1.392(4) yes
C8 C9 . 1.379(5) yes
C8 H8 . 0.93 ?
C9 C10 . 1.378(6) yes
C9 H9 . 0.93 ?
C10 C11 . 1.387(4) yes
C10 H10 . 0.93 ?
C11 H11 . 0.93 ?