#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/29/2212963.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_2212963
loop_
_publ_author_name
'Nichol, Gary S.'
'Clegg, William'
_publ_section_title
;
 A synchrotron study of
 catena-poly[[tri-μ-aqua-triaquabarium(II)]
 bis(6-methylpyridin-2-olate)]
;
_journal_coeditor_code           LH2341
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1135
_journal_page_last               m1137
_journal_paper_doi               10.1107/S1600536807013037
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ba (H2 O)6] (C6 H6 N O)2'
_chemical_formula_moiety         'H12 Ba O6 2+, 2(C6 H6 N O -)'
_chemical_formula_sum            'C12 H24 Ba N2 O8'
_chemical_formula_weight         461.67
_chemical_name_systematic
;
catena-poly[[tri-μ-aqua-triaquabarium(II)] bis(6-methylpyridin-2-olate)]
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6080(9)
_cell_length_b                   30.353(3)
_cell_length_c                   7.8280(10)
_cell_measurement_reflns_used    6905
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.1
_cell_measurement_theta_min      3.50
_cell_volume                     1807.7(4)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2004)'
_computing_publication_material
;
SHELXTL, publCIF (Westrip, 2007) and local programs
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2001)'
_computing_structure_solution    'SIR97 (Altomare et al.,  1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'Thin-slice ω'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6751
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13751
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.20
_diffrn_reflns_theta_min         3.55
_diffrn_standards_decay_%        10
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.235
_exptl_absorpt_correction_T_max  0.807
_exptl_absorpt_correction_T_min  0.689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.835
_refine_diff_density_min         -2.911
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.215
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2834
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.214
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0439
_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)+(0.0225P)²+12.2343P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1048
_reflns_number_gt                2513
_reflns_number_total             2834
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            lh2341.cif
_cod_data_source_block           I
_cod_database_code               2212963
_cod_database_fobs_code          2212963
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
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 0.53740(5) 0.2500 0.11370(4) 0.01415(10) Uani d S 1
O O1 1.0231(4) 0.16785(10) -0.0562(4) 0.0194(6) Uani d . 1
O O2 0.7751(7) 0.2500 -0.1473(6) 0.0276(10) Uani d SD 1
H H2O 0.808(8) 0.2717(13) -0.198(7) 0.033 Uiso d D 1
O O3 0.4537(6) 0.18705(12) -0.1176(5) 0.0356(9) Uani d D 1
H H3OA 0.394(8) 0.1664(16) -0.087(8) 0.043 Uiso d D 1
H H3OB 0.494(8) 0.182(2) -0.213(5) 0.043 Uiso d D 1
O O4 0.8119(4) 0.18951(10) 0.2079(4) 0.0193(6) Uani d D 1
H H4OA 0.868(7) 0.1814(17) 0.124(5) 0.023 Uiso d D 1
H H4OB 0.796(7) 0.1706(18) 0.269(6) 0.023 Uiso d D 1
O O5 0.6598(6) 0.2500 0.4516(5) 0.0169(8) Uani d SD 1
H H5O 0.632(7) 0.2720(12) 0.499(6) 0.020 Uiso d D 1
N N1 1.2377(5) 0.12034(12) 0.0322(4) 0.0192(7) Uani d . 1
C C1 1.0820(6) 0.12755(13) -0.0475(5) 0.0173(7) Uani d . 1
C C2 0.9888(6) 0.09184(14) -0.1222(5) 0.0224(8) Uani d . 1
H H2 0.8795 0.0968 -0.1779 0.027 Uiso calc R 1
C C3 1.0581(7) 0.05007(15) -0.1132(6) 0.0261(9) Uani d . 1
H H3 0.9968 0.0260 -0.1629 0.031 Uiso calc R 1
C C4 1.2186(7) 0.04304(14) -0.0312(6) 0.0255(9) Uani d . 1
H H4 1.2677 0.0143 -0.0244 0.031 Uiso calc R 1
C C5 1.3048(6) 0.07880(14) 0.0402(5) 0.0217(8) Uani d . 1
C C6 1.4797(7) 0.07435(18) 0.1274(7) 0.0335(11) Uani d . 1
H H6A 1.5642 0.0946 0.0746 0.050 Uiso calc R 1
H H6B 1.5221 0.0440 0.1156 0.050 Uiso calc R 1
H H6C 1.4671 0.0815 0.2488 0.050 Uiso calc R 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
O2 Ba O3 . . 69.83(11)
O2 Ba O3 . 8_565 69.83(11)
O2 Ba O4 . . 73.18(11)
O2 Ba O4 . 3_455 139.41(6)
O2 Ba O4 . 6_556 139.40(6)
O2 Ba O4 . 8_565 73.18(11)
O2 Ba O5 . . 119.09(15)
O2 Ba O5 . 6_556 121.43(14)
O3 Ba O3 . 8_565 89.75(19)
O3 Ba O4 . . 83.78(12)
O3 Ba O4 . 3_455 129.43(12)
O3 Ba O4 8_565 3_455 74.57(10)
O3 Ba O4 . 6_556 74.57(10)
O3 Ba O4 8_565 6_556 129.43(12)
O3 Ba O4 . 8_565 142.40(10)
O3 Ba O4 8_565 8_565 83.78(12)
O3 Ba O4 8_565 . 142.40(10)
O3 Ba O5 . . 135.12(9)
O3 Ba O5 8_565 . 135.12(9)
O3 Ba O5 . 6_556 69.60(11)
O3 Ba O5 8_565 6_556 69.60(11)
O4 Ba O4 3_455 6_556 79.38(12)
O4 Ba O4 3_455 8_565 84.33(7)
O4 Ba O4 6_556 8_565 135.75(4)
O4 Ba O4 . 3_455 135.75(4)
O4 Ba O4 . 6_556 84.33(7)
O4 Ba O4 . 8_565 79.32(13)
O4 Ba O5 . . 61.13(8)
O4 Ba O5 3_455 . 74.93(9)
O4 Ba O5 6_556 . 74.93(9)
O4 Ba O5 8_565 . 61.13(8)
O4 Ba O5 3_455 6_556 59.84(8)
O4 Ba O5 6_556 6_556 59.84(8)
O4 Ba O5 8_565 6_556 139.43(7)
O4 Ba O5 . 6_556 139.43(7)
O5 Ba O5 . 6_556 119.48(11)
Ba O2 H2O . . 125(4)
Ba O3 H3OA . . 119(4)
Ba O3 H3OB . . 131(4)
H3OA O3 H3OB . . 109(5)
Ba O4 Ba . 6_656 98.63(9)
Ba O4 H4OA . . 111(4)
Ba O4 H4OA 6_656 . 105(4)
Ba O4 H4OB . . 122(4)
Ba O4 H4OB 6_656 . 106(4)
H4OA O4 H4OB . . 111(5)
Ba O5 Ba . 6_656 99.30(13)
Ba O5 H5O . . 111(4)
Ba O5 H5O 6_656 . 110(4)
C1 N1 C5 . . 119.9(4)
O1 C1 N1 . . 118.4(4)
O1 C1 C2 . . 121.5(4)
N1 C1 C2 . . 120.1(4)
C1 C2 H2 . . 120.3
C1 C2 C3 . . 119.4(4)
H2 C2 C3 . . 120.3
C2 C3 H3 . . 120.0
C2 C3 C4 . . 120.0(4)
H3 C3 C4 . . 120.0
C3 C4 H4 . . 120.7
C3 C4 C5 . . 118.7(4)
H4 C4 C5 . . 120.7
N1 C5 C4 . . 121.9(4)
N1 C5 C6 . . 115.9(4)
C4 C5 C6 . . 122.2(4)
C5 C6 H6A . . 109.5
C5 C6 H6B . . 109.5
C5 C6 H6C . . 109.5
H6A C6 H6B . . 109.5
H6A C6 H6C . . 109.5
H6B C6 H6C . . 109.5
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
Ba O2 . 2.729(5) yes
Ba O3 . 2.708(3) yes
Ba O3 8_565 2.708(3) ?
Ba O4 . 2.877(3) yes
Ba O4 3_455 2.875(3) yes
Ba O4 6_556 2.875(3) ?
Ba O4 8_565 2.877(3) ?
Ba O5 . 2.804(4) yes
Ba O5 6_556 2.918(4) yes
O1 C1 . 1.305(5) yes
O2 H2O . 0.81(3) ?
O3 H3OA . 0.81(3) ?
O3 H3OB . 0.82(3) ?
O4 Ba 6_656 2.875(3) ?
O4 H4OA . 0.82(2) ?
O4 H4OB . 0.76(5) ?
O5 Ba 6_656 2.918(4) ?
O5 H5O . 0.79(3) ?
N1 C1 . 1.357(5) yes
N1 C5 . 1.362(5) yes
C1 C2 . 1.421(6) yes
C2 H2 . 0.9500 ?
C2 C3 . 1.375(6) yes
C3 H3 . 0.950 ?
C3 C4 . 1.396(7) yes
C4 H4 . 0.950 ?
C4 C5 . 1.386(6) yes
C5 C6 . 1.501(7) yes
C6 H6A . 0.980 ?
C6 H6B . 0.980 ?
C6 H6C . 0.980 ?
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
_geom_hbond_publ_flag
O2 H2O O3 3_554 0.81(3) 2.21(3) 2.981(6) 160(6) yes
O3 H3OA N1 1_455 0.81(3) 2.06(3) 2.859(5) 170(6) yes
O3 H3OB O1 6 0.82(3) 1.87(3) 2.672(5) 165(6) yes
O4 H4OA O1 . 0.82(2) 1.88(2) 2.699(4) 172(6) yes
O4 H4OB N1 6_556 0.76(5) 2.23(5) 2.977(5) 174(5) yes
O5 H5O O1 3_455 0.79(3) 2.06(3) 2.823(4) 163(5) yes
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
O2 Ba O4 Ba . 6_656 90.70(11)
O3 Ba O4 Ba . 6_656 161.47(11)
O3 Ba O4 Ba 8_565 6_656 80.03(19)
O4 Ba O4 Ba 3_455 6_656 -55.05(15)
O4 Ba O4 Ba 6_556 6_656 -123.49(13)
O4 Ba O4 Ba 8_565 6_656 15.21(12)
O5 Ba O4 Ba . 6_656 -47.59(9)
O5 Ba O4 Ba 6_556 6_656 -150.31(13)
Ba Ba O5 Ba 6_556 6_656 180.0
O2 Ba O5 Ba . 6_656 0.0
O3 Ba O5 Ba . 6_656 89.98(15)
O3 Ba O5 Ba 8_565 6_656 -89.98(15)
O4 Ba O5 Ba 3_455 6_656 -138.59(6)
O4 Ba O5 Ba 6_556 6_656 138.59(6)
O4 Ba O5 Ba 8_565 6_656 -46.79(8)
O4 Ba O5 Ba . 6_656 46.79(8)
O5 Ba O5 Ba 6_556 6_656 180.0
C5 N1 C1 O1 . . -178.6(4)
C5 N1 C1 C2 . . 0.2(6)
O1 C1 C2 C3 . . 178.5(4)
N1 C1 C2 C3 . . -0.2(6)
C1 C2 C3 C4 . . 0.1(7)
C2 C3 C4 C5 . . 0.1(7)
C1 N1 C5 C4 . . 0.0(6)
C1 N1 C5 C6 . . 178.6(4)
C3 C4 C5 N1 . . -0.1(7)
C3 C4 C5 C6 . . -178.6(4)
