#------------------------------------------------------------------------------
#$Date: 2019-11-07 12:44:57 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223448 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/21/52/2215220.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_2215220
loop_
_publ_author_name
'Peng-Zhi Hong'
'Wen-Dong Song'
'Zao-He Wu'
_publ_section_title
;
 Poly[[tetra-μ₂-aqua-diaqua-μ₆-oxalato-barium(II)]
 2,4,6-trinitrophenolate monohydrate]
;
_journal_coeditor_code           LX2010
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2296
_journal_page_last               m2296
_journal_paper_doi               10.1107/S1600536807038159
_journal_volume                  63
_journal_year                    2007
_chemical_formula_sum            'C14 H24 Ba2 N6 O28'
_chemical_formula_weight         999.08
_chemical_name_systematic
;Poly[[tetra-μ₂-aqua-diaqua-μ₆-oxalato-barium(II)]
 2,4,6-trinitrophenolate
monohydrate]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 93.5570(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.1489(2)
_cell_length_b                   6.57360(10)
_cell_length_c                   15.3111(2)
_cell_measurement_reflns_used    3600
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      1.66
_cell_volume                     1521.79(4)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2004)'
_computing_publication_material  'SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII 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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13176
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.67
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.695
_exptl_absorpt_correction_T_max  0.650
_exptl_absorpt_correction_T_min  0.608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.530
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         3654
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0237
_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)+(0.0277P)²+0.4903P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0523
_refine_ls_wR_factor_ref         0.0555
_reflns_number_gt                3126
_reflns_number_total             3654
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            lx2010.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-11-07
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C7 H12 Ba N3 O14'
_cod_original_formula_weight         499.54
_cod_original_formula_moiety         'C H8 Ba O6 +, C6 H2 N3 O7 -, H2 O'
_cod_original_formula_iupac          '[Ba (C2 O4) (H2 O)6] C6 H2 N3 O7, H2 O'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        1521.78(4)
_cod_original_sg_symbol_Hall     -p_2ybc
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2215220
_cod_database_fobs_code          2215220
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Ba Ba 0.009199(10) 0.090317(19) 0.144062(9) 0.02169(6) Uani d . 1
C C1 0.53089(19) 0.0665(4) 0.32517(18) 0.0287(6) Uani d . 1
H H1 0.5152 0.0558 0.3828 0.034 Uiso calc R 1
C C2 0.61794(18) 0.0706(4) 0.30611(17) 0.0272(6) Uani d . 1
C C3 0.64955(18) 0.0795(4) 0.21936(17) 0.0264(6) Uani d . 1
C C4 0.57696(19) 0.0866(4) 0.15341(17) 0.0286(6) Uani d . 1
C C5 0.48959(19) 0.0906(4) 0.17056(18) 0.0291(6) Uani d . 1
H H5 0.4462 0.1012 0.1251 0.035 Uiso calc R 1
C C6 0.46645(18) 0.0786(4) 0.25682(18) 0.0266(6) Uani d . 1
C C7 -0.00848(17) 0.4258(3) -0.03987(16) 0.0215(5) Uani d . 1
H H1WA 0.182(2) -0.021(3) 0.4331(19) 0.026 Uiso d D 1
H H1WB 0.2387(13) 0.113(4) 0.4163(19) 0.026 Uiso d D 1
H H2WA 0.0900(16) -0.317(4) 0.1881(15) 0.026 Uiso d D 1
H H2WB 0.1540(11) -0.240(4) 0.2382(17) 0.026 Uiso d D 1
H H3WA 0.1313(16) 0.224(4) 0.3221(14) 0.026 Uiso d D 1
H H3WB 0.1543(15) 0.353(4) 0.2658(17) 0.026 Uiso d D 1
H H4WA 0.2140(16) 0.102(4) 0.1052(16) 0.026 Uiso d D 1
H H4WB 0.1765(18) 0.208(3) 0.0395(15) 0.026 Uiso d D 1
H H5WA -0.2039(15) 0.144(4) 0.1023(15) 0.026 Uiso d D 1
H H5WB -0.1725(18) 0.123(4) 0.0273(12) 0.026 Uiso d D 1
N N1 0.68199(17) 0.0555(4) 0.38123(16) 0.0374(6) Uani d . 1
N N2 0.37473(16) 0.0789(3) 0.27700(17) 0.0349(6) Uani d . 1
N N3 0.59676(18) 0.0979(4) 0.06088(16) 0.0386(6) Uani d . 1
O O1 0.73001(13) 0.0796(3) 0.20391(13) 0.0393(5) Uani d . 1
O O2 0.75026(17) 0.1514(5) 0.38100(16) 0.0711(8) Uani d . 1
O O3 0.66196(17) -0.0536(4) 0.44163(15) 0.0607(7) Uani d . 1
O O4 0.35790(16) 0.0651(4) 0.35365(16) 0.0553(7) Uani d . 1
O O5 0.31768(15) 0.0929(4) 0.21685(17) 0.0556(7) Uani d . 1
O O6 0.54645(17) 0.1997(4) 0.01244(15) 0.0593(7) Uani d . 1
O O7 0.65884(16) 0.0004(5) 0.03584(15) 0.0611(7) Uani d . 1
O O8 -0.00452(12) 0.2386(2) -0.02508(10) 0.0256(4) Uani d . 1
O O9 0.02537(13) 0.4939(3) 0.11302(11) 0.0311(4) Uani d . 1
O O1W 0.18547(15) 0.1042(4) 0.42656(16) 0.0439(5) Uani d D 1
O O2W 0.10105(13) -0.2370(3) 0.22765(12) 0.0294(4) Uani d D 1
O O3W 0.11131(13) 0.2932(3) 0.28179(13) 0.0322(4) Uani d D 1
O O4W 0.17396(15) 0.1144(3) 0.07199(16) 0.0432(5) Uani d D 1
O O5W -0.16202(14) 0.1761(4) 0.07469(14) 0.0397(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'
Ba Ba -0.3244 2.2819 '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
O9 Ba O8 . . 59.49(5)
O9 Ba O4W . . 77.44(6)
O8 Ba O4W . . 68.10(6)
O9 Ba O5W . . 80.09(6)
O8 Ba O5W . . 63.84(6)
O4W Ba O5W . . 131.91(6)
O9 Ba O2W . . 141.07(6)
O8 Ba O2W . . 134.40(5)
O4W Ba O2W . . 78.19(6)
O5W Ba O2W . . 138.08(6)
O9 Ba O8 . 3 129.44(5)
O8 Ba O8 . 3 70.63(5)
O4W Ba O8 . 3 77.07(6)
O5W Ba O8 . 3 85.63(6)
O2W Ba O8 . 3 72.61(5)
O9 Ba O3W . . 67.85(5)
O8 Ba O3W . . 122.09(5)
O4W Ba O3W . . 79.03(6)
O5W Ba O3W . . 129.11(6)
O2W Ba O3W . . 78.05(5)
O8 Ba O3W 3 . 145.21(5)
O9 Ba O2W . 2 78.28(6)
O8 Ba O2W . 2 119.06(5)
O4W Ba O2W . 2 144.51(6)
O5W Ba O2W . 2 67.51(6)
O2W Ba O2W . 2 106.29(4)
O8 Ba O2W 3 2 138.31(5)
O3W Ba O2W . 2 67.99(5)
O9 Ba O3W . 2_545 141.37(6)
O8 Ba O3W . 2_545 125.61(5)
O4W Ba O3W . 2_545 141.16(6)
O5W Ba O3W . 2_545 72.43(6)
O2W Ba O3W . 2_545 67.69(6)
O8 Ba O3W 3 2_545 75.52(5)
O3W Ba O3W . 2_545 110.10(3)
O2W Ba O3W 2 2_545 66.46(5)
C2 C1 C6 . . 118.7(3)
C1 C2 C3 . . 125.3(2)
C1 C2 N1 . . 115.6(2)
C3 C2 N1 . . 119.1(2)
O1 C3 C2 . . 123.7(2)
O1 C3 C4 . . 125.0(3)
C2 C3 C4 . . 111.3(2)
C5 C4 C3 . . 124.8(3)
C5 C4 N3 . . 116.3(2)
C3 C4 N3 . . 118.9(3)
C4 C5 C6 . . 119.1(2)
C1 C6 C5 . . 120.8(3)
C1 C6 N2 . . 118.7(3)
C5 C6 N2 . . 120.5(2)
O9 C7 O8 3_565 . 125.6(2)
O9 C7 C7 3_565 3_565 116.6(2)
O8 C7 C7 . 3_565 117.8(2)
O2 N1 O3 . . 124.0(3)
O2 N1 C2 . . 119.2(2)
O3 N1 C2 . . 116.8(2)
O4 N2 O5 . . 123.2(3)
O4 N2 C6 . . 117.9(2)
O5 N2 C6 . . 118.9(3)
O7 N3 O6 . . 123.9(3)
O7 N3 C4 . . 119.0(3)
O6 N3 C4 . . 117.0(3)
H1WA O1W H1WB . . 99(3)
H2WA O2W H2WB . . 107(2)
H3WA O3W H3WB . . 104(2)
H4WA O4W H4WB . . 116(2)
H5WA O5W H5WB . . 104(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ba O9 . 2.709(2)
Ba O8 . 2.763(2)
Ba O4W . 2.795(2)
Ba O5W . 2.799(2)
Ba O2W . 2.825(2)
Ba O8 3 2.826(2)
Ba O3W . 2.866(2)
Ba O2W 2 2.888(2)
Ba O3W 2_545 2.949(2)
Ba Ba 565 6.957(3)
Ba Ba 3 4.5603(3)
Ba Ba 2 4.6386(2)
Ba Ba 2_545 4.6386(2)
C1 C2 . 1.368(4)
C1 C6 . 1.388(4)
C1 H1 . 0.9300
C2 C3 . 1.441(4)
C2 N1 . 1.461(3)
C3 O1 . 1.256(3)
C3 C4 . 1.447(4)
C4 C5 . 1.366(4)
C4 N3 . 1.468(4)
C5 C6 . 1.390(4)
C5 H5 . 0.9300
C6 N2 . 1.442(4)
C7 O9 3_565 1.250(3)
C7 O8 . 1.252(3)
C7 C7 3_565 1.571(5)
N1 O2 . 1.212(3)
N1 O3 . 1.223(3)
N2 O4 . 1.220(3)
N2 O5 . 1.227(3)
N3 O7 . 1.219(3)
N3 O6 . 1.228(3)
O1W H1WA . 0.832(17)
O1W H1WB . 0.834(17)
O2W H2WA . 0.810(16)
O2W H2WB . 0.809(16)
O3W H3WA . 0.808(16)
O3W H3WB . 0.813(16)
O4W H4WA . 0.771(16)
O4W H4WB . 0.796(16)
O5W H5WA . 0.812(16)
O5W H5WB . 0.812(16)
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
O1W H1WB O4 . 0.834(17) 2.12(2) 2.915(3) 159(3)
O1W H1WA O5W 2_545 0.832(17) 2.016(18) 2.837(3) 169(3)
O2W H2WB O1 2_645 0.809(16) 2.25(2) 2.961(3) 146(3)
O2W H2WB O2 2_645 0.809(16) 2.50(3) 2.974(3) 118(2)
O2W H2WA O9 1_545 0.810(16) 1.922(16) 2.697(3) 160(3)
O3W H3WB O1 2_655 0.813(16) 2.32(2) 3.051(3) 149(3)
O3W H3WA O1W . 0.808(16) 1.922(17) 2.722(3) 170(3)
O4W H4WA O5 . 0.771(16) 2.250(17) 3.013(3) 171(3)
O4W H4WB O1W 4_565 0.796(16) 2.134(17) 2.908(3) 164(3)
O5W H5WA O1 1_455 0.812(16) 1.948(17) 2.719(3) 158(3)
O5W H5WA O7 1_455 0.812(16) 2.45(2) 2.975(3) 124(2)
O5W H5WB O4W 3 0.812(16) 2.178(18) 2.945(3) 158(3)
