#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/37/2013710.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_2013710
loop_
_publ_author_name
'Kolitsch, Uwe'
_publ_section_title
;
 Two bismuth oxalate hydrates and revision of their chemical formulae
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m501
_journal_page_last               m504
_journal_paper_doi               10.1107/S0108270103023618
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Bi2 (C2 O4)3 (H2 O)4], 4H2 O'
_chemical_formula_moiety         'Bi2 (C2 O4)3 (H2 O)8'
_chemical_formula_sum            'C6 H16 Bi2 O20'
_chemical_formula_weight         826.15
_chemical_name_common            'bismuth oxalate octahydrate'
_chemical_name_systematic
;
tetraaquatri-μ-oxalato-dibismuth(III) tetrahydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                101.15(3)
_cell_angle_beta                 101.76(3)
_cell_angle_gamma                106.17(3)
_cell_formula_units_Z            2
_cell_length_a                   9.194(2)
_cell_length_b                   9.458(2)
_cell_length_c                   11.176(2)
_cell_measurement_reflns_used    5313
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.577
_cell_measurement_theta_min      2.037
_cell_volume                     880.9(4)
_computing_cell_refinement       'HKL SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2002)'
_computing_data_reduction
'HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK'
_computing_molecular_graphics    'ATOMS (Shape Software, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10808
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.61
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.055
_exptl_absorpt_correction_T_max  0.5845
_exptl_absorpt_correction_T_min  0.1229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(HKL SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.115
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.727
_refine_diff_density_min         -1.866
_refine_ls_extinction_coef       0.0050(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         6122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0276
_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)+(0.029P)²+0.6P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0671
_reflns_number_gt                4981
_reflns_number_total             6122
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ta1420.cif
_cod_data_source_block           II
_cod_database_code               2013710
_cod_database_fobs_code          2013710
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Bi1 0.238507(17) 0.658354(17) 0.126577(14) 0.01630(5) Uani d . 1 . . Bi
Bi2 0.080104(17) 0.885970(17) -0.356471(14) 0.01648(5) Uani d . 1 . . Bi
C1 0.2371(5) 0.7895(5) -0.1128(4) 0.0172(8) Uani d . 1 . . C
C2 0.0704(5) 0.6693(5) -0.1595(4) 0.0183(8) Uani d . 1 . . C
C3 -0.0776(5) 1.0839(5) -0.1980(4) 0.0181(8) Uani d . 1 . . C
C4 -0.0835(5) 1.1511(5) -0.3150(4) 0.0169(8) Uani d . 1 . . C
C5 0.6123(5) 0.8086(5) 0.2301(4) 0.0182(8) Uani d . 1 . . C
C6 0.5465(5) 0.9224(5) 0.3020(4) 0.0191(8) Uani d . 1 . . C
O1 0.2684(4) 0.8872(4) -0.1726(3) 0.0279(7) Uani d . 1 . . O
O2 0.3331(4) 0.7833(4) -0.0169(3) 0.0238(7) Uani d . 1 . . O
O3 0.0332(4) 0.5809(4) -0.0925(3) 0.0226(6) Uani d . 1 . . O
O4 -0.0146(3) 0.6709(4) -0.2620(3) 0.0238(7) Uani d . 1 . . O
O5 -0.1094(4) 1.1524(4) -0.1050(3) 0.0285(8) Uani d . 1 . . O
O6 -0.0408(4) 0.9656(4) -0.2023(3) 0.0266(7) Uani d . 1 . . O
O7 -0.1115(4) 1.2743(4) -0.3041(3) 0.0265(7) Uani d . 1 . . O
O8 -0.0594(4) 1.0767(4) -0.4096(3) 0.0212(6) Uani d . 1 . . O
O9 0.7583(4) 0.8484(4) 0.2476(3) 0.0260(7) Uani d . 1 . . O
O10 0.5146(4) 0.6832(4) 0.1601(3) 0.0251(7) Uani d . 1 . . O
O11 0.6417(4) 1.0370(4) 0.3831(3) 0.0265(7) Uani d . 1 . . O
O12 0.3984(4) 0.8859(4) 0.2737(3) 0.0265(7) Uani d . 1 . . O
OW1 -0.1963(4) 0.7271(4) -0.4784(4) 0.0359(9) Uani d . 1 . . O
OW2 0.2659(5) 0.4210(5) -0.0195(4) 0.0450(10) Uani d . 1 . . O
OW3 0.3098(4) 0.5299(4) 0.3032(3) 0.0264(7) Uani d . 1 . . O
OW4 0.1190(5) 0.6471(4) -0.4747(4) 0.0379(9) Uani d . 1 . . O
OW5 0.4763(5) 0.3419(5) 0.2638(4) 0.0483(11) Uani d . 1 . . O
OW6 0.4911(4) 0.2400(4) 0.4788(4) 0.0380(9) Uani d . 1 . . O
OW7 0.7728(5) 0.5271(5) 0.2982(4) 0.0514(11) Uani d . 1 . . O
OW8A 0.330(6) 0.142(2) 0.054(2) 0.043(8) Uani d P 0.31(6) . . O
OW8B 0.249(3) 0.1533(13) 0.0451(8) 0.056(5) Uani d P 0.69(6) . . 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi -4.1077 10.2566 '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
O12 Bi1 O2 . . 82.98(12)
O12 Bi1 O10 . . 68.74(11)
O2 Bi1 O10 . . 72.08(11)
O12 Bi1 O5 . 2_575 72.54(12)
O2 Bi1 O5 . 2_575 72.66(11)
O10 Bi1 O5 . 2_575 129.82(12)
O12 Bi1 O7 . 2_575 69.07(11)
O2 Bi1 O7 . 2_575 134.58(11)
O10 Bi1 O7 . 2_575 124.44(12)
O5 Bi1 O7 2_575 2_575 65.27(11)
O12 Bi1 OW3 . . 85.67(12)
O2 Bi1 OW3 . . 144.74(11)
O10 Bi1 OW3 . . 72.69(11)
O5 Bi1 OW3 2_575 . 134.45(11)
O7 Bi1 OW3 2_575 . 69.70(11)
O12 Bi1 O3 . . 135.90(12)
O2 Bi1 O3 . . 67.04(10)
O10 Bi1 O3 . . 125.57(11)
O5 Bi1 O3 2_575 . 68.16(11)
O7 Bi1 O3 2_575 . 109.83(11)
OW3 Bi1 O3 . . 136.96(10)
O12 Bi1 OW2 . . 139.05(12)
O2 Bi1 OW2 . . 83.47(13)
O10 Bi1 OW2 . . 70.34(13)
O5 Bi1 OW2 2_575 . 137.89(13)
O7 Bi1 OW2 2_575 . 140.43(13)
OW3 Bi1 OW2 . . 83.57(13)
O3 Bi1 OW2 . . 70.74(13)
O12 Bi1 O3 . 2_565 140.09(11)
O2 Bi1 O3 . 2_565 130.95(10)
O10 Bi1 O3 . 2_565 134.30(10)
O5 Bi1 O3 2_575 2_565 95.85(11)
O7 Bi1 O3 2_575 2_565 71.41(11)
OW3 Bi1 O3 . 2_565 75.71(10)
O3 Bi1 O3 . 2_565 64.51(11)
OW2 Bi1 O3 . 2_565 74.10(12)
O6 Bi2 O1 . . 81.65(12)
O6 Bi2 O9 . 2_675 74.46(12)
O1 Bi2 O9 . 2_675 71.81(12)
O6 Bi2 O4 . . 71.33(11)
O1 Bi2 O4 . . 66.14(11)
O9 Bi2 O4 2_675 . 128.50(11)
O6 Bi2 OW1 . . 83.20(13)
O1 Bi2 OW1 . . 136.42(12)
O9 Bi2 OW1 2_675 . 140.93(12)
O4 Bi2 OW1 . . 70.30(12)
O6 Bi2 OW4 . . 140.83(12)
O1 Bi2 OW4 . . 88.27(13)
O9 Bi2 OW4 2_675 . 137.34(12)
O4 Bi2 OW4 . . 69.98(12)
OW1 Bi2 OW4 . . 78.44(13)
O6 Bi2 O11 . 2_675 135.59(12)
O1 Bi2 O11 . 2_675 68.82(11)
O9 Bi2 O11 2_675 2_675 65.35(11)
O4 Bi2 O11 . 2_675 120.84(11)
OW1 Bi2 O11 . 2_675 140.77(11)
OW4 Bi2 O11 . 2_675 72.37(13)
O6 Bi2 O8 . . 66.73(10)
O1 Bi2 O8 . . 133.50(11)
O9 Bi2 O8 2_675 . 67.51(11)
O4 Bi2 O8 . . 127.31(10)
OW1 Bi2 O8 . . 74.36(12)
OW4 Bi2 O8 . . 137.56(11)
O11 Bi2 O8 2_675 . 111.35(11)
O6 Bi2 O8 . 2_574 131.09(10)
O1 Bi2 O8 . 2_574 141.05(10)
O9 Bi2 O8 2_675 2_574 94.92(11)
O4 Bi2 O8 . 2_574 136.57(10)
OW1 Bi2 O8 . 2_574 76.06(12)
OW4 Bi2 O8 . 2_574 77.12(11)
O11 Bi2 O8 2_675 2_574 72.35(11)
O8 Bi2 O8 . 2_574 65.17(11)
O1 C1 O2 . . 124.0(4)
O1 C1 C2 . . 117.5(4)
O2 C1 C2 . . 118.5(4)
O3 C2 O4 . . 126.5(4)
O3 C2 C1 . . 117.6(4)
O4 C2 C1 . . 115.9(4)
O5 C3 O6 . . 123.9(4)
O5 C3 C4 . . 117.6(4)
O6 C3 C4 . . 118.5(4)
O8 C4 O7 . . 126.8(4)
O8 C4 C3 . . 116.7(4)
O7 C4 C3 . . 116.6(4)
O9 C5 O10 . . 125.6(4)
O9 C5 C6 . . 117.1(4)
O10 C5 C6 . . 117.3(4)
O11 C6 O12 . . 126.2(4)
O11 C6 C5 . . 117.9(4)
O12 C6 C5 . . 115.9(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
Bi1 O12 . 2.320(3) yes
Bi1 O2 . 2.335(3) yes
Bi1 O10 . 2.426(3) yes
Bi1 O5 2_575 2.430(3) yes
Bi1 O7 2_575 2.564(3) yes
Bi1 OW3 . 2.577(3) yes
Bi1 O3 . 2.597(3) yes
Bi1 OW2 . 2.614(4) yes
Bi1 O3 2_565 2.763(3) yes
Bi2 O6 . 2.349(3) yes
Bi2 O1 . 2.398(3) yes
Bi2 O9 2_675 2.450(3) yes
Bi2 O4 . 2.496(3) yes
Bi2 OW1 . 2.498(4) yes
Bi2 OW4 . 2.543(4) yes
Bi2 O11 2_675 2.553(3) yes
Bi2 O8 . 2.577(3) yes
Bi2 O8 2_574 2.681(3) yes
C1 O1 . 1.246(5) yes
C1 O2 . 1.265(5) yes
C1 C2 . 1.545(6) yes
C2 O3 . 1.251(5) yes
C2 O4 . 1.253(5) yes
C3 O5 . 1.247(5) yes
C3 O6 . 1.251(5) yes
C3 C4 . 1.557(6) yes
C4 O8 . 1.248(5) yes
C4 O7 . 1.251(5) yes
C5 O9 . 1.250(5) yes
C5 O10 . 1.260(5) yes
C5 C6 . 1.548(6) yes
C6 O11 . 1.237(5) yes
C6 O12 . 1.262(5) yes
OW6 Bi1 2_666 4.372(4) ?
OW6 Bi2 2_665 4.797(4) ?
OW7 Bi2 1_656 4.421(5) ?
OW7 Bi2 2_665 4.592(5) ?
OW7 Bi1 2_665 4.701(5) ?
OW8A OW8B . 0.77(2) ?
OW8A Bi2 1_545 4.52(3) ?
OW8A Bi1 1_545 4.676(18) ?
OW8B Bi2 1_545 4.420(9) ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
O1 C1 C2 O3 -172.9(4)
O2 C1 C2 O3 7.1(6)
O1 C1 C2 O4 6.9(6)
O2 C1 C2 O4 -173.1(4)
O5 C3 C4 O8 -176.4(4)
O6 C3 C4 O8 3.9(6)
O5 C3 C4 O7 3.8(6)
O6 C3 C4 O7 -175.9(4)
O9 C5 C6 O11 -8.3(6)
O10 C5 C6 O11 170.9(4)
O9 C5 C6 O12 173.6(4)
O10 C5 C6 O12 -7.2(6)
