#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/86/2218630.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_2218630
loop_
_publ_author_name
'Hao, Lujiang'
'Mu, Chunhua'
'Wang, Ridong'
_publ_section_title
;Tetraaquabis[(1-carboxylatomethyl-1,3-benzimidazol-3-ium-3-yl)acetato-κO]palladium(II)
 dihydrate
;
_journal_coeditor_code           CF2196
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m896
_journal_paper_doi               10.1107/S1600536808016097
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Pd (C11 H9 N2 O4)2 (H2 O)4], 2H2 O'
_chemical_formula_moiety         'C22 H26 N4 O12 Pd, 2 H2 O'
_chemical_formula_sum            'C22 H30 N4 O14 Pd'
_chemical_formula_weight         680.90
_chemical_name_systematic
;
Tetraaquabis[(1-carboxylatomethyl-1,3-benzimidazol-3-ium-3-yl)acetato-
\kO]palladium(II) dihydrate
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.13(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.4702(10)
_cell_length_b                   11.794(2)
_cell_length_c                   20.886(3)
_cell_measurement_reflns_used    2425
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.20
_cell_measurement_theta_min      1.96
_cell_volume                     1342.1(4)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7075
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  0.8489
_exptl_absorpt_correction_T_min  0.7331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.488
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2425
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0420P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0723
_reflns_number_gt                1958
_reflns_number_total             2425
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cf2196.cif
_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_enum 1527 2010-12-29 10:47:43Z saulius 

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_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2218630
_cod_database_fobs_code          2218630
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_type_symbol
_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
Pd Pd1 0.5000 1.0000 0.0000 0.02449(11) Uani d S 1
C C1 0.7711(5) 1.0484(2) 0.14648(12) 0.0299(6) Uani d . 1
C C2 0.5544(5) 0.9924(2) 0.17543(12) 0.0326(6) Uani d . 1
H H2A 0.4065 1.0354 0.1631 0.039 Uiso calc R 1
H H2B 0.5316 0.9166 0.1578 0.039 Uiso calc R 1
C C3 0.4539(5) 1.0371(2) 0.28620(12) 0.0294(6) Uani d . 1
H H3 0.3237 1.0858 0.2745 0.035 Uiso calc R 1
C C4 0.7676(4) 0.9208(2) 0.28035(12) 0.0279(6) Uani d . 1
C C5 0.9568(5) 0.8536(2) 0.26202(14) 0.0365(7) Uani d . 1
H H5 0.9834 0.8433 0.2190 0.044 Uiso calc R 1
C C6 1.1029(6) 0.8030(3) 0.31070(17) 0.0480(8) Uani d . 1
H H6 1.2346 0.7586 0.3006 0.058 Uiso calc R 1
C C7 1.0587(6) 0.8166(3) 0.37470(17) 0.0540(9) Uani d . 1
H H7 1.1595 0.7793 0.4062 0.065 Uiso calc R 1
C C8 0.8726(6) 0.8828(3) 0.39307(15) 0.0449(7) Uani d . 1
H H8 0.8444 0.8916 0.4360 0.054 Uiso calc R 1
C C9 0.7282(5) 0.9361(2) 0.34427(12) 0.0299(6) Uani d . 1
C C11 0.4355(5) 1.0558(3) 0.40327(13) 0.0369(7) Uani d . 1
H H11A 0.4276 0.9955 0.4346 0.044 Uiso calc R 1
H H11B 0.2696 1.0831 0.3923 0.044 Uiso calc R 1
C C12 0.5910(5) 1.1527(2) 0.43369(13) 0.0347(6) Uani d . 1
H H1W 0.545(5) 0.681(2) 0.2365(7) 0.042 Uiso d D 1
H H2W 0.571(4) 0.693(2) 0.1719(9) 0.042 Uiso d D 1
H H3W 0.160(5) 1.1619(14) 0.0196(13) 0.042 Uiso d D 1
H H4W 0.074(4) 1.078(2) 0.0568(12) 0.042 Uiso d D 1
H H5W 0.503(3) 0.7896(18) 0.0589(13) 0.042 Uiso d D 1
H H6W 0.270(3) 0.799(2) 0.0290(13) 0.042 Uiso d D 1
N N1 0.5889(4) 0.98516(17) 0.24523(11) 0.0290(5) Uani d . 1
N N2 0.5306(4) 1.01001(17) 0.34575(11) 0.0301(5) Uani d . 1
O O1 0.1897(3) 1.09974(17) 0.03739(10) 0.0394(5) Uani d D 1
O O2 0.3926(4) 0.83292(17) 0.04423(10) 0.0451(5) Uani d D 1
O O3 0.7682(3) 1.03890(18) 0.08641(9) 0.0384(5) Uani d . 1
O O4 0.9339(4) 1.09448(18) 0.18150(9) 0.0460(5) Uani d . 1
O O5 0.7726(4) 1.1842(2) 0.40763(11) 0.0650(7) Uani d . 1
O O6 0.5172(3) 1.19231(18) 0.48365(9) 0.0439(5) Uani d . 1
O O7 0.4821(4) 0.7010(2) 0.20114(10) 0.0485(5) Uani d D 1
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'
S S 0.1246 0.1234 '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
O1 Pd1 O1 . 3_675 180.00(9)
O1 Pd1 O3 . . 94.14(7)
O1 Pd1 O3 3_675 . 85.86(8)
O1 Pd1 O3 . 3_675 85.86(8)
O1 Pd1 O3 3_675 3_675 94.14(7)
O3 Pd1 O3 . 3_675 180.0
O1 Pd1 O2 . 3_675 85.34(7)
O1 Pd1 O2 3_675 3_675 94.66(7)
O3 Pd1 O2 . 3_675 88.61(7)
O3 Pd1 O2 3_675 3_675 91.39(7)
O1 Pd1 O2 . . 94.66(7)
O1 Pd1 O2 3_675 . 85.34(7)
O3 Pd1 O2 . . 91.39(7)
O3 Pd1 O2 3_675 . 88.61(7)
O2 Pd1 O2 3_675 . 180.00(10)
O4 C1 O3 . . 125.3(2)
O4 C1 C2 . . 120.2(2)
O3 C1 C2 . . 114.5(2)
N1 C2 C1 . . 112.7(2)
N1 C2 H2A . . 109.1
C1 C2 H2A . . 109.1
N1 C2 H2B . . 109.1
C1 C2 H2B . . 109.1
H2A C2 H2B . . 107.8
N2 C3 N1 . . 110.3(2)
N2 C3 H3 . . 124.8
N1 C3 H3 . . 124.8
C9 C4 C5 . . 121.8(2)
C9 C4 N1 . . 106.0(2)
C5 C4 N1 . . 132.3(2)
C6 C5 C4 . . 116.4(3)
C6 C5 H5 . . 121.8
C4 C5 H5 . . 121.8
C5 C6 C7 . . 121.5(3)
C5 C6 H6 . . 119.2
C7 C6 H6 . . 119.2
C8 C7 C6 . . 122.4(3)
C8 C7 H7 . . 118.8
C6 C7 H7 . . 118.8
C7 C8 C9 . . 116.3(3)
C7 C8 H8 . . 121.8
C9 C8 H8 . . 121.8
C8 C9 C4 . . 121.6(3)
C8 C9 N2 . . 131.4(3)
C4 C9 N2 . . 106.9(2)
N2 C11 C12 . . 113.2(2)
N2 C11 H11A . . 108.9
C12 C11 H11A . . 108.9
N2 C11 H11B . . 108.9
C12 C11 H11B . . 108.9
H11A C11 H11B . . 107.7
O5 C12 O6 . . 126.3(3)
O5 C12 C11 . . 118.9(2)
O6 C12 C11 . . 114.8(2)
C3 N1 C4 . . 108.4(2)
C3 N1 C2 . . 126.0(2)
C4 N1 C2 . . 125.5(2)
C3 N2 C9 . . 108.3(2)
C3 N2 C11 . . 125.6(2)
C9 N2 C11 . . 125.9(2)
Pd1 O1 H3W . . 115.2(18)
Pd1 O1 H4W . . 130.4(18)
H3W O1 H4W . . 111(2)
Pd1 O2 H5W . . 118.6(19)
Pd1 O2 H6W . . 120.1(19)
H5W O2 H6W . . 112(2)
C1 O3 Pd1 . . 139.53(17)
H1W O7 H2W . . 114(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Pd1 O1 . 2.2608(19)
Pd1 O1 3_675 2.2608(19)
Pd1 O3 . 2.2687(19)
Pd1 O3 3_675 2.2687(19)
Pd1 O2 3_675 2.276(2)
Pd1 O2 . 2.276(2)
C1 O4 . 1.227(3)
C1 O3 . 1.258(3)
C1 C2 . 1.529(4)
C2 N1 . 1.456(3)
C2 H2A . 0.970
C2 H2B . 0.970
C3 N2 . 1.316(4)
C3 N1 . 1.329(3)
C3 H3 . 0.930
C4 C9 . 1.383(3)
C4 C5 . 1.384(4)
C4 N1 . 1.394(3)
C5 C6 . 1.373(4)
C5 H5 . 0.930
C6 C7 . 1.389(4)
C6 H6 . 0.930
C7 C8 . 1.364(5)
C7 H7 . 0.930
C8 C9 . 1.383(4)
C8 H8 . 0.930
C9 N2 . 1.392(3)
C11 N2 . 1.455(3)
C11 C12 . 1.528(4)
C11 H11A . 0.970
C11 H11B . 0.970
C12 O5 . 1.232(3)
C12 O6 . 1.243(3)
O1 H3W . 0.832(10)
O1 H4W . 0.823(10)
O2 H5W . 0.828(10)
O2 H6W . 0.824(10)
O7 H1W . 0.822(10)
O7 H2W . 0.821(10)
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
O7 H1W O4 2_645 0.822(10) 1.985(14) 2.756(3) 156(3)
O7 H2W O5 2_645 0.821(10) 1.937(10) 2.747(3) 169(3)
