#------------------------------------------------------------------------------
#$Date: 2017-03-27 08:13:23 +0300 (Mon, 27 Mar 2017) $
#$Revision: 194538 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/01/40/2014024.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_2014024
loop_
_publ_author_name
'Vertruyen, Bénédicte'
'Robertz, Bénédicte'
'Guillaume, Bernard'
'Rulmont, André'
'Spirlet, Marie-Rose'
_publ_section_title
;
 Dibarium zirconium tetraoxalate trihydrate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m233
_journal_page_last               m234
_journal_paper_doi               10.1107/S0108270104006791
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Ba2 Zr (C2 O4)4 (H2 O)3]'
_chemical_formula_moiety         'C8 H6 Ba2 O19 Zr'
_chemical_formula_structural     'Ba2 Zr (C2 O4)4 , 3H2 O'
_chemical_formula_sum            'C8 H6 Ba2 O19 Zr'
_chemical_formula_weight         772.03
_chemical_name_common            'Barium zirconium oxalate hydrate'
_chemical_name_systematic
;
Triaquatetraoxalatodibarium(II)zirconium(IV)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   undef
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 115.45(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2010(12)
_cell_length_b                   29.032(5)
_cell_length_c                   9.2079(17)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.23
_cell_measurement_theta_min      4.90
_cell_volume                     2221.0(8)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        'SHELXTL (Siemens, 1991)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       2θ/ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6582
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.049
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.907
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.309
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.047
_refine_diff_density_min         -0.799
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         1964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.038P)²+45.4129P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1244
_reflns_number_gt                1510
_reflns_number_total             1964
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            iz1040.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-03-27

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2221.0(7)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               2014024
_cod_database_fobs_code          2014024
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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
_atom_site_attached_hydrogens
Ba1 0.2500 0.47133(3) 0.5000 0.0227(3) Uani d S 1 . . Ba 0
Ba2 -0.2500 0.22910(3) 1.0000 0.0319(3) Uani d S 1 . . Ba 0
Zr1 0.2500 0.38452(4) 1.0000 0.0190(3) Uani d S 1 . . Zr 0
O1 -0.1750(8) 0.4651(3) 0.7752(9) 0.0380(18) Uani d . 1 . . O 0
O2 -0.0175(9) 0.4593(3) 0.5776(8) 0.0344(17) Uani d . 1 . . O 0
O3 0.1784(8) 0.4234(2) 0.7784(8) 0.0269(15) Uani d . 1 . . O 0
O4 0.0308(8) 0.4247(3) 0.9569(8) 0.0315(16) Uani d . 1 . . O 0
O5 0.1468(8) 0.3497(2) 1.1474(8) 0.0281(15) Uani d . 1 . . O 0
O6 0.0697(9) 0.3355(3) 0.8494(8) 0.0354(18) Uani d . 1 . . O 0
O7 -0.1188(10) 0.2843(3) 0.8289(9) 0.0402(19) Uani d . 1 . . O 0
O8 -0.0490(14) 0.3039(4) 1.1453(11) 0.074(3) Uani d . 1 . . O 0
O9W -0.0259(10) 0.4438(4) 0.2333(10) 0.067(3) Uani d . 1 . . O 2
O10W 0.2500 0.3756(5) 0.5000 0.079(5) Uani d S 1 . . O 2
C1 -0.0473(12) 0.4455(3) 0.8221(12) 0.025(2) Uani d . 1 . . C 0
C2 0.0432(12) 0.4432(3) 0.7134(12) 0.024(2) Uani d . 1 . . C 0
C3 0.0273(13) 0.3227(4) 1.0819(13) 0.036(3) Uani d . 1 . . C 0
C4 -0.0133(13) 0.3124(4) 0.9048(13) 0.033(2) Uani d . 1 . . C 0
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 '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'
H H 0.0000 0.0000 '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
O10W Ba1 O9W . . 73.3(2) no
O10W Ba1 O9W . 2_556 73.3(2) no
O9W Ba1 O9W . 2_556 146.6(5) no
O10W Ba1 O2 . 6_665 136.04(16) no
O9W Ba1 O2 . 6_665 137.6(3) no
O9W Ba1 O2 2_556 6_665 71.0(3) no
O10W Ba1 O2 . 5_566 136.04(16) no
O9W Ba1 O2 . 5_566 71.0(3) no
O9W Ba1 O2 2_556 5_566 137.6(3) no
O2 Ba1 O2 6_665 5_566 87.9(3) no
O10W Ba1 O2 . 2_556 82.98(16) no
O9W Ba1 O2 . 2_556 107.5(2) no
O9W Ba1 O2 2_556 2_556 68.3(2) no
O2 Ba1 O2 6_665 2_556 60.5(3) no
O2 Ba1 O2 5_566 2_556 131.98(18) no
O10W Ba1 O2 . . 82.98(16) no
O9W Ba1 O2 . . 68.3(2) no
O9W Ba1 O2 2_556 . 107.5(2) no
O2 Ba1 O2 6_665 . 131.98(18) no
O2 Ba1 O2 5_566 . 60.5(3) no
O2 Ba1 O2 2_556 . 166.0(3) no
O10W Ba1 O1 . 6_665 128.49(16) no
O9W Ba1 O1 . 6_665 136.2(2) no
O9W Ba1 O1 2_556 6_665 68.7(3) no
O2 Ba1 O1 6_665 6_665 57.46(19) no
O2 Ba1 O1 5_566 6_665 69.0(2) no
O2 Ba1 O1 2_556 6_665 112.30(19) no
O2 Ba1 O1 . 6_665 76.9(2) no
O10W Ba1 O1 . 5_566 128.49(16) no
O9W Ba1 O1 . 5_566 68.7(3) no
O9W Ba1 O1 2_556 5_566 136.2(2) no
O2 Ba1 O1 6_665 5_566 69.0(2) no
O2 Ba1 O1 5_566 5_566 57.46(19) no
O2 Ba1 O1 2_556 5_566 76.9(2) no
O2 Ba1 O1 . 5_566 112.30(19) no
O1 Ba1 O1 6_665 5_566 103.0(3) no
O10W Ba1 O3 . 2_556 64.43(12) no
O9W Ba1 O3 . 2_556 66.1(2) no
O9W Ba1 O3 2_556 2_556 99.0(3) no
O2 Ba1 O3 6_665 2_556 96.82(18) no
O2 Ba1 O3 5_566 2_556 120.18(19) no
O2 Ba1 O3 2_556 2_556 42.07(18) no
O2 Ba1 O3 . 2_556 129.56(19) no
O1 Ba1 O3 6_665 2_556 153.59(17) no
O1 Ba1 O3 5_566 2_556 69.01(19) no
O10W Ba1 O3 . . 64.43(12) no
O9W Ba1 O3 . . 99.0(3) no
O9W Ba1 O3 2_556 . 66.1(2) no
O2 Ba1 O3 6_665 . 120.18(19) no
O2 Ba1 O3 5_566 . 96.82(18) no
O2 Ba1 O3 2_556 . 129.56(19) no
O2 Ba1 O3 . . 42.07(18) no
O1 Ba1 O3 6_665 . 69.01(19) no
O1 Ba1 O3 5_566 . 153.59(17) no
O3 Ba1 O3 2_556 . 128.9(2) no
O10W Ba1 C2 . 2_556 75.97(16) no
O9W Ba1 C2 . 2_556 86.9(2) no
O9W Ba1 C2 2_556 2_556 85.1(3) no
O2 Ba1 C2 6_665 2_556 76.2(2) no
O2 Ba1 C2 5_566 2_556 125.9(2) no
O2 Ba1 C2 2_556 2_556 20.6(2) no
O2 Ba1 C2 . 2_556 151.3(2) no
O1 Ba1 C2 6_665 2_556 131.8(2) no
O1 Ba1 C2 5_566 2_556 68.6(2) no
O3 Ba1 C2 2_556 2_556 21.9(2) no
O3 Ba1 C2 . 2_556 135.9(2) no
O7 Ba2 O7 7_456 8 163.8(3) no
O7 Ba2 O8 7_456 . 121.5(3) no
O7 Ba2 O8 8 . 72.4(3) no
O7 Ba2 O8 7_456 2_457 72.4(3) no
O7 Ba2 O8 8 2_457 121.5(3) no
O8 Ba2 O8 . 2_457 77.9(5) no
O7 Ba2 O7 7_456 . 64.1(3) no
O7 Ba2 O7 8 . 126.5(3) no
O8 Ba2 O7 . . 58.5(2) no
O8 Ba2 O7 2_457 . 69.4(3) no
O7 Ba2 O7 7_456 2_457 126.5(3) no
O7 Ba2 O7 8 2_457 64.1(3) no
O8 Ba2 O7 . 2_457 69.4(3) no
O8 Ba2 O7 2_457 2_457 58.5(2) no
O7 Ba2 O7 . 2_457 111.6(3) no
O7 Ba2 Ba2 7_456 7_456 32.64(16) no
O7 Ba2 Ba2 8 7_456 156.08(18) no
O8 Ba2 Ba2 . 7_456 89.42(19) no
O8 Ba2 Ba2 2_457 7_456 67.27(18) no
O7 Ba2 Ba2 . 7_456 31.49(15) no
O7 Ba2 Ba2 2_457 7_456 124.49(15) no
O7 Ba2 Ba2 7_456 7_457 156.08(18) no
O7 Ba2 Ba2 8 7_457 32.64(16) no
O8 Ba2 Ba2 . 7_457 67.27(18) no
O8 Ba2 Ba2 2_457 7_457 89.42(19) no
O7 Ba2 Ba2 . 7_457 124.49(15) no
O7 Ba2 Ba2 2_457 7_457 31.49(15) no
Ba2 Ba2 Ba2 7_456 7_457 150.47(4) no
O3 Zr1 O3 2_557 . 117.4(4) no
O3 Zr1 O6 2_557 . 141.3(2) no
O3 Zr1 O6 . . 84.3(3) no
O3 Zr1 O6 2_557 2_557 84.3(3) no
O3 Zr1 O6 . 2_557 141.3(2) no
O6 Zr1 O6 . 2_557 98.2(4) no
O3 Zr1 O5 2_557 2_557 141.1(3) no
O3 Zr1 O5 . 2_557 72.4(2) no
O6 Zr1 O5 . 2_557 73.7(3) no
O6 Zr1 O5 2_557 2_557 71.4(2) no
O3 Zr1 O5 2_557 . 72.4(2) no
O3 Zr1 O5 . . 141.1(3) no
O6 Zr1 O5 . . 71.4(2) no
O6 Zr1 O5 2_557 . 73.7(3) no
O5 Zr1 O5 2_557 . 125.4(4) no
O3 Zr1 O4 2_557 2_557 70.9(2) no
O3 Zr1 O4 . 2_557 77.3(3) no
O6 Zr1 O4 . 2_557 147.8(3) no
O6 Zr1 O4 2_557 2_557 81.0(3) no
O5 Zr1 O4 2_557 2_557 75.6(3) no
O5 Zr1 O4 . 2_557 137.0(2) no
O3 Zr1 O4 2_557 . 77.3(3) no
O3 Zr1 O4 . . 70.9(2) no
O6 Zr1 O4 . . 81.0(3) no
O6 Zr1 O4 2_557 . 147.8(3) no
O5 Zr1 O4 2_557 . 137.0(2) no
O5 Zr1 O4 . . 75.6(3) no
O4 Zr1 O4 2_557 . 116.4(4) no
C1 O1 O9W . 2_456 134.8(7) no
C1 O1 Ba1 . 5_566 115.6(6) no
O9W O1 Ba1 2_456 5_566 104.4(3) no
C2 O2 Ba1 . 5_566 120.0(6) no
C2 O2 Ba1 . . 103.8(6) no
Ba1 O2 Ba1 5_566 . 119.5(3) no
C2 O3 Zr1 . . 121.4(6) no
C2 O3 Ba1 . . 85.6(5) no
Zr1 O3 Ba1 . . 152.7(3) no
C1 O4 Zr1 . . 120.6(6) no
C1 O4 O9W . 1_556 121.8(6) no
Zr1 O4 O9W . 1_556 116.3(3) no
C3 O5 Zr1 . . 120.2(6) no
C3 O5 O10W . 1_556 117.8(6) no
Zr1 O5 O10W . 1_556 121.3(3) no
C4 O6 Zr1 . . 120.9(6) no
C4 O7 Ba2 . 7_456 125.6(7) no
C4 O7 Ba2 . . 118.5(6) no
Ba2 O7 Ba2 7_456 . 115.9(3) no
C3 O8 Ba2 . . 121.2(8) no
Ba1 O9W O1 . 2_456 118.4(3) no
Ba1 O9W O4 . 1_554 113.2(3) no
O1 O9W O4 2_456 1_554 124.9(4) no
Ba1 O9W O10W . . 53.3(3) no
O1 O9W O10W 2_456 . 125.8(4) no
O4 O9W O10W 1_554 . 99.7(3) no
Ba1 O10W O5 . 1_554 104.3(3) no
Ba1 O10W O5 . 2_557 104.3(3) no
O5 O10W O5 1_554 2_557 151.5(6) no
Ba1 O10W O9W . 2_556 53.4(3) no
O5 O10W O9W 1_554 2_556 136.2(3) no
O5 O10W O9W 2_557 2_556 64.7(2) no
O1 C1 O4 . . 128.4(9) no
O1 C1 C2 . . 119.9(9) no
O4 C1 C2 . . 111.7(8) no
O2 C2 O3 . . 125.7(9) no
O2 C2 C1 . . 120.4(9) no
O3 C2 C1 . . 113.9(8) no
O2 C2 Ba1 . . 55.6(5) no
O3 C2 Ba1 . . 72.5(5) no
C1 C2 Ba1 . . 163.3(6) no
O8 C3 O5 . . 127.4(10) no
O8 C3 C4 . . 119.7(10) no
O5 C3 C4 . . 112.9(9) no
O7 C4 O6 . . 125.7(10) no
O7 C4 C3 . . 120.2(9) no
O6 C4 C3 . . 114.1(9) no
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
Ba1 O10W . 2.778(14) yes
Ba1 O9W . 2.785(8) yes
Ba1 O9W 2_556 2.785(8) no
Ba1 O2 6_665 2.799(7) yes
Ba1 O2 5_566 2.799(7) no
Ba1 O2 2_556 2.864(7) no
Ba1 O2 . 2.864(7) yes
Ba1 O1 6_665 2.968(7) yes
Ba1 O1 5_566 2.968(7) no
Ba1 O3 2_556 3.224(6) no
Ba1 O3 . 3.224(6) yes
Ba1 C2 2_556 3.370(9) no
Ba2 O7 7_456 2.764(7) yes
Ba2 O7 8 2.764(7) no
Ba2 O8 . 2.793(9) yes
Ba2 O8 2_457 2.793(9) no
Ba2 O7 . 2.854(8) yes
Ba2 O7 2_457 2.854(8) no
Ba2 Ba2 7_456 4.7612(9) no
Ba2 Ba2 7_457 4.7612(10) no
Zr1 O3 2_557 2.172(6) no
Zr1 O3 . 2.172(6) yes
Zr1 O6 . 2.173(7) yes
Zr1 O6 2_557 2.173(7) no
Zr1 O5 2_557 2.209(6) no
Zr1 O5 . 2.209(6) yes
Zr1 O4 2_557 2.213(7) no
Zr1 O4 . 2.213(7) yes
O1 C1 . 1.205(12) no
O1 O9W 2_456 2.789(11) no
O1 Ba1 5_566 2.968(7) no
O2 C2 . 1.222(12) no
O2 Ba1 5_566 2.799(7) no
O3 C2 . 1.263(11) no
O4 C1 . 1.287(12) no
O4 O9W 1_556 2.863(11) no
O5 C3 . 1.272(12) no
O5 O10W 1_556 3.059(7) no
O6 C4 . 1.277(12) no
O7 C4 . 1.230(13) no
O7 Ba2 7_456 2.764(7) no
O8 C3 . 1.218(14) no
O9W O1 2_456 2.789(11) yes
O9W O4 1_554 2.863(11) yes
O9W O10W . 3.321(14) no
O10W O5 1_554 3.059(7) yes
O10W O5 2_557 3.059(7) no
O10W O9W 2_556 3.321(14) no
C1 C2 . 1.555(13) no
C3 C4 . 1.537(15) no
