#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/76/2217616.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_2217616
loop_
_publ_author_name
'Chongzhen Mei'
'Kaihui Li'
'Peng Zhang'
_publ_section_title
;Poly[[tetraaquabis(1H-imidazole-κN³)bis[2-(oxaloamino)benzoato(3--)]dicopper(II)barium(II)]
 dihydrate]
;
_journal_coeditor_code           PK2076
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m356
_journal_page_last               m356
_journal_paper_doi               10.1107/S1600536808000597
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac
'[Ba Cu2 (C9 H4 N O5)2 (C3 H4 N2)2 (H2 O)4] , 2H2 O'
_chemical_formula_moiety         'C24 H24 Ba Cu2 N6 O14 , 2H2 O'
_chemical_formula_sum            'C24 H28 Ba Cu2 N6 O16'
_chemical_formula_weight         920.94
_chemical_name_systematic
;
Poly[[tetraaquabis(1H-imidazole-\kN³)bis[2-
(oxaloamino)benzoato(3-)]dicopper(II)barium(II)] dihydrate]
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 101.146(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.662(3)
_cell_length_b                   6.9165(18)
_cell_length_c                   21.335(5)
_cell_measurement_reflns_used    857
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.331
_cell_measurement_theta_min      2.945
_cell_volume                     1543.6(7)
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  'publCIF (Westrip, 2008)'
_computing_structure_refinement  'SHELXTL (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART 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  0.0838
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7263
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.713
_exptl_absorpt_correction_T_max  0.583
_exptl_absorpt_correction_T_min  0.525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.981
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.855
_refine_diff_density_min         -0.645
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         2713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.04P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0892
_reflns_number_gt                2398
_reflns_number_total             2713
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            pk2076.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               2217616
_cod_database_fobs_code          2217616
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ba Ba1 0.5000 0.90568(5) 0.7500 0.03268(14) Uani d S 1 . .
Cu Cu2 0.70008(4) 0.79877(8) 1.03715(2) 0.03358(16) Uani d . 1 . .
C C1 0.4210(4) 0.7210(6) 0.9961(2) 0.0308(9) Uani d . 1 . .
C C2 0.3109(4) 0.6829(7) 0.9499(2) 0.0413(10) Uani d . 1 . .
H H2 0.3156 0.6890 0.9069 0.050 Uiso calc R 1 . .
C C3 0.1959(4) 0.6366(7) 0.9667(2) 0.0459(12) Uani d . 1 . .
H H3 0.1245 0.6136 0.9350 0.055 Uiso calc R 1 . .
C C4 0.1856(4) 0.6243(7) 1.0289(2) 0.0460(12) Uani d . 1 . .
H H4 0.1082 0.5917 1.0401 0.055 Uiso calc R 1 . .
C C5 0.2922(4) 0.6609(7) 1.0754(2) 0.0415(10) Uani d . 1 . .
H H5 0.2856 0.6533 1.1182 0.050 Uiso calc R 1 . .
C C6 0.4103(4) 0.7096(6) 1.0598(2) 0.0334(9) Uani d . 1 . .
C C7 0.5146(4) 0.7449(7) 1.1180(2) 0.0362(10) Uani d . 1 . .
C C8 1.0359(4) 0.7848(9) 1.1711(2) 0.0550(14) Uani d . 1 . .
H H8 1.0897 0.7403 1.2078 0.066 Uiso calc R 1 . .
C C9 0.9614(4) 0.9421(7) 1.0840(2) 0.0464(12) Uani d . 1 . .
H H9 0.9563 1.0274 1.0499 0.056 Uiso calc R 1 . .
C C10 0.9169(4) 0.7209(8) 1.1470(2) 0.0479(12) Uani d . 1 . .
H H10 0.8736 0.6250 1.1648 0.058 Uiso calc R 1 . .
C C12 0.5519(4) 0.7837(6) 0.91832(19) 0.0345(10) Uani d . 1 . .
C C13 0.6890(4) 0.8380(7) 0.91134(19) 0.0339(9) Uani d . 1 . .
N N1 0.5387(3) 0.7682(5) 0.97887(15) 0.0301(7) Uani d . 1 . .
N N2 0.8704(3) 0.8215(6) 1.09186(17) 0.0390(8) Uani d . 1 . .
N N3 1.0623(3) 0.9254(6) 1.13173(18) 0.0484(10) Uani d . 1 . .
H H3A 1.1315 0.9922 1.1365 0.058 Uiso calc R 1 . .
O O1 0.7097(3) 0.8641(5) 0.85734(13) 0.0460(8) Uani d . 1 . .
O O2 0.4736(3) 0.7653(6) 0.86823(14) 0.0549(10) Uani d . 1 . .
O O3 0.7724(2) 0.8539(5) 0.96263(13) 0.0412(7) Uani d . 1 . .
O O4 0.6293(3) 0.7678(5) 1.11137(13) 0.0466(8) Uani d . 1 . .
O O5 0.7323(3) 1.0322(6) 0.72527(16) 0.0648(10) Uani d . 1 . .
H H5B 0.7114 1.0964 0.6909 0.097 Uiso d R 1 . .
H H5C 0.7768 0.9304 0.7246 0.097 Uiso d R 1 . .
O O8 0.4863(3) 0.7515(5) 1.17116(14) 0.0462(8) Uani d . 1 . .
O O9 0.3581(4) 0.5293(6) 0.7463(2) 0.0893(13) Uani d . 1 . .
H H9C 0.2794 0.5576 0.7421 0.134 Uiso d R 1 . .
H H9A 0.3773 0.4384 0.7804 0.134 Uiso d R 1 . .
O O10 0.874(3) 0.681(4) 0.7671(15) 0.143(6) Uani d P 0.44(2) A 1
O O10' 0.8713(19) 0.711(3) 0.7229(13) 0.143(6) Uani d P 0.56(2) A 2
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'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
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
O2 Ba1 O2 2_656 . 138.93(16)
O2 Ba1 O5 2_656 . 71.64(10)
O2 Ba1 O5 . . 122.44(9)
O2 Ba1 O5 2_656 2_656 122.44(9)
O2 Ba1 O5 . 2_656 71.64(10)
O5 Ba1 O5 . 2_656 143.21(18)
O2 Ba1 O1 2_656 2_656 56.10(8)
O2 Ba1 O1 . 2_656 119.20(9)
O5 Ba1 O1 . 2_656 117.63(9)
O5 Ba1 O1 2_656 2_656 66.37(9)
O2 Ba1 O1 2_656 . 119.20(9)
O2 Ba1 O1 . . 56.10(8)
O5 Ba1 O1 . . 66.37(9)
O5 Ba1 O1 2_656 . 117.63(9)
O1 Ba1 O1 2_656 . 168.57(15)
O2 Ba1 O8 2_656 3_677 144.53(10)
O2 Ba1 O8 . 3_677 76.13(10)
O5 Ba1 O8 . 3_677 84.57(10)
O5 Ba1 O8 2_656 3_677 65.01(10)
O1 Ba1 O8 2_656 3_677 119.12(9)
O1 Ba1 O8 . 3_677 71.12(10)
O2 Ba1 O8 2_656 4_575 76.13(10)
O2 Ba1 O8 . 4_575 144.53(10)
O5 Ba1 O8 . 4_575 65.01(10)
O5 Ba1 O8 2_656 4_575 84.57(10)
O1 Ba1 O8 2_656 4_575 71.12(10)
O1 Ba1 O8 . 4_575 119.12(9)
O8 Ba1 O8 3_677 4_575 69.99(12)
O2 Ba1 O9 2_656 . 79.15(11)
O2 Ba1 O9 . . 65.19(11)
O5 Ba1 O9 . . 137.09(13)
O5 Ba1 O9 2_656 . 79.31(13)
O1 Ba1 O9 2_656 . 65.44(11)
O1 Ba1 O9 . . 104.07(11)
O8 Ba1 O9 3_677 . 133.93(10)
O8 Ba1 O9 4_575 . 136.55(10)
O2 Ba1 O9 2_656 2_656 65.19(11)
O2 Ba1 O9 . 2_656 79.15(11)
O5 Ba1 O9 . 2_656 79.31(13)
O5 Ba1 O9 2_656 2_656 137.09(13)
O1 Ba1 O9 2_656 2_656 104.07(11)
O1 Ba1 O9 . 2_656 65.44(11)
O8 Ba1 O9 3_677 2_656 136.55(10)
O8 Ba1 O9 4_575 2_656 133.93(10)
O9 Ba1 O9 . 2_656 59.89(18)
O4 Cu2 N1 . . 94.38(13)
O4 Cu2 O3 . . 175.12(15)
N1 Cu2 O3 . . 86.53(13)
O4 Cu2 N2 . . 89.12(13)
N1 Cu2 N2 . . 175.91(14)
O3 Cu2 N2 . . 90.17(13)
C6 C1 C2 . . 117.4(3)
C6 C1 N1 . . 120.9(4)
C2 C1 N1 . . 121.7(4)
C3 C2 C1 . . 121.7(4)
C3 C2 H2 . . 119.1
C1 C2 H2 . . 119.1
C4 C3 C2 . . 120.9(4)
C4 C3 H3 . . 119.6
C2 C3 H3 . . 119.6
C3 C4 C5 . . 118.7(4)
C3 C4 H4 . . 120.6
C5 C4 H4 . . 120.6
C4 C5 C6 . . 121.7(4)
C4 C5 H5 . . 119.1
C6 C5 H5 . . 119.1
C1 C6 C5 . . 119.5(4)
C1 C6 C7 . . 127.3(3)
C5 C6 C7 . . 113.2(4)
O8 C7 O4 . . 120.8(4)
O8 C7 C6 . . 119.3(3)
O4 C7 C6 . . 119.9(3)
C10 C8 N3 . . 107.1(4)
C10 C8 H8 . . 126.5
N3 C8 H8 . . 126.5
N2 C9 N3 . . 110.7(4)
N2 C9 H9 . . 124.6
N3 C9 H9 . . 124.6
C8 C10 N2 . . 108.5(4)
C8 C10 H10 . . 125.8
N2 C10 H10 . . 125.8
O2 C12 N1 . . 130.9(4)
O2 C12 C13 . . 116.0(3)
N1 C12 C13 . . 113.1(3)
O1 C13 O3 . . 124.8(4)
O1 C13 C12 . . 118.2(3)
O3 C13 C12 . . 117.0(3)
C12 N1 C1 . . 122.5(3)
C12 N1 Cu2 . . 111.6(3)
C1 N1 Cu2 . . 125.8(3)
C9 N2 C10 . . 106.1(4)
C9 N2 Cu2 . . 126.5(3)
C10 N2 Cu2 . . 127.3(3)
C9 N3 C8 . . 107.6(4)
C9 N3 H3A . . 126.2
C8 N3 H3A . . 126.2
C13 O1 Ba1 . . 120.4(2)
C12 O2 Ba1 . . 125.8(3)
C13 O3 Cu2 . . 111.5(2)
C7 O4 Cu2 . . 131.0(3)
C7 O8 Ba1 . 3_677 124.9(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ba1 O2 2_656 2.767(3)
Ba1 O2 . 2.767(3)
Ba1 O5 . 2.772(3)
Ba1 O5 2_656 2.772(3)
Ba1 O1 2_656 2.889(3)
Ba1 O1 . 2.889(3)
Ba1 O8 3_677 2.894(3)
Ba1 O8 4_575 2.894(3)
Ba1 O9 . 3.004(5)
Ba1 O9 2_656 3.004(4)
Cu2 O4 . 1.894(3)
Cu2 N1 . 1.930(3)
Cu2 O3 . 1.934(3)
Cu2 N2 . 1.966(3)
C1 C6 . 1.389(6)
C1 C2 . 1.404(6)
C1 N1 . 1.412(5)
C2 C3 . 1.380(6)
C2 H2 . 0.9300
C3 C4 . 1.355(7)
C3 H3 . 0.9300
C4 C5 . 1.379(6)
C4 H4 . 0.9300
C5 C6 . 1.404(5)
C5 H5 . 0.9300
C6 C7 . 1.518(6)
C7 O8 . 1.230(5)
C7 O4 . 1.268(5)
C8 C10 . 1.347(6)
C8 N3 . 1.349(6)
C8 H8 . 0.9300
C9 N2 . 1.314(6)
C9 N3 . 1.335(6)
C9 H9 . 0.9300
C10 N2 . 1.375(6)
C10 H10 . 0.9300
C12 O2 . 1.229(5)
C12 N1 . 1.331(5)
C12 C13 . 1.544(5)
C13 O1 . 1.228(5)
C13 O3 . 1.274(5)
N3 H3A . 0.8600
O5 H5B . 0.8502
O5 H5C . 0.8500
O8 Ba1 3_677 2.894(3)
O9 H9C . 0.8498
O9 H9A . 0.9530
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
N3 H3A O1 3_777 0.86 1.95 2.804(5) 177
O5 H5B O4 4_575 0.85 1.99 2.827(5) 169
O5 H5B O8 4_575 0.85 2.58 3.047(5) 116
O9 H9A O8 3_667 0.95 2.08 2.915(5) 145
