#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/80/2018021.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_2018021
loop_
_publ_author_name
'Stavila, Vitalie'
'Bulimestru, Ion'
'Gulea, Aurelian'
'Colson, Adam C.'
'Whitmire, Kenton H.'
_publ_section_title
;
 Hexaaquacobalt(II) and hexaaquanickel(II)
 bis(μ-pyridine-2,6-dicarboxylato)bis[(pyridine-2,6-dicarboxylato)bismuthate(III)]
 dihydrate
;
_journal_coeditor_code           SQ3274
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m65
_journal_page_last               m68
_journal_paper_doi               10.1107/S0108270110053497
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Co (H2 O)6] [Bi2 (C7 H4 N O4)4] , 2H2 O'
_chemical_formula_moiety         'H12 Co1 O6 2+, C27 H16 Bi2 N4 O16 2-, 2H2 O'
_chemical_formula_sum            'C28 H28 Bi2 Co N4 O24'
_chemical_formula_weight         1281.43
_chemical_name_systematic
;
hexaaquacobalt(II) bis(μ-pyridine-2,6-dicarboxylato)bis[(pyridine-2,6-
dicarboxylato)bismuthate(III)] dihydrate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                112.99(3)
_cell_angle_beta                 90.67(3)
_cell_angle_gamma                97.44(3)
_cell_formula_units_Z            1
_cell_length_a                   7.2966(15)
_cell_length_b                   11.184(2)
_cell_length_c                   12.004(2)
_cell_measurement_reflns_used    9400
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.65
_cell_measurement_theta_min      2.82
_cell_volume                     892.1(4)
_computing_cell_refinement       'XSCANS (Bruker, 1997)'
_computing_data_collection       'XSCANS (Bruker, 1997)'
_computing_data_reduction        'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'Bruker CCD 1000 area-detector'
_diffrn_measurement_method       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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10685
_diffrn_reflns_theta_full        28.54
_diffrn_reflns_theta_max         28.54
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    10.403
_exptl_absorpt_correction_T_max  0.3941
_exptl_absorpt_correction_T_min  0.2186
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            light-pink
_exptl_crystal_density_diffrn    2.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             609
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.100
_refine_diff_density_min         -1.725
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         4176
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0244
_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)+(0.0304P)²+1.1642P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0634
_reflns_number_gt                3914
_reflns_number_total             4176
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sq3274.cif
_cod_data_source_block           I
_cod_original_cell_volume        892.1(3)
_cod_database_code               2018021
_cod_database_fobs_code          2018021
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi Bi1 0.389333(19) 0.311936(13) 0.371001(12) 0.02241(6) Uani d . 1 . .
N N1 0.3445(5) 0.2102(3) 0.5221(3) 0.0242(7) Uani d . 1 . .
N N2 0.5785(5) 0.2340(3) 0.2057(3) 0.0234(7) Uani d . 1 . .
O O11 0.4431(5) 0.4703(3) 0.6070(3) 0.0318(7) Uani d . 1 . .
O O12 0.4744(5) 0.4851(3) 0.7978(3) 0.0353(7) Uani d . 1 . .
O O13 0.3068(5) 0.0871(3) 0.2822(3) 0.0331(7) Uani d . 1 . .
O O14 0.2018(6) -0.1019(3) 0.2943(3) 0.0454(9) Uani d . 1 . .
O O21 0.2421(4) 0.2833(3) 0.1716(3) 0.0288(6) Uani d . 1 . .
O O22 0.2624(5) 0.2020(4) -0.0287(3) 0.0467(9) Uani d . 1 . .
O O23 0.6765(4) 0.2977(3) 0.4349(3) 0.0325(7) Uani d . 1 . .
O O24 0.9639(5) 0.2571(4) 0.3941(3) 0.0455(9) Uani d . 1 . .
C C11 0.4371(6) 0.4224(4) 0.6881(4) 0.0269(8) Uani d . 1 . .
C C12 0.3773(6) 0.2763(4) 0.6420(4) 0.0253(8) Uani d . 1 . .
C C13 0.3537(7) 0.2131(4) 0.7204(4) 0.0319(9) Uani d . 1 . .
H H13A 0.3811 0.2596 0.8033 0.038 Uiso calc R 1 . .
C C14 0.2895(8) 0.0816(5) 0.6751(4) 0.0428(12) Uani d . 1 . .
H H14A 0.2685 0.0384 0.7271 0.051 Uiso calc R 1 . .
C C15 0.2561(8) 0.0134(5) 0.5511(4) 0.0387(11) Uani d . 1 . .
H H15A 0.2141 -0.0763 0.5183 0.046 Uiso calc R 1 . .
C C16 0.2866(6) 0.0815(4) 0.4770(4) 0.0272(8) Uani d . 1 . .
C C17 0.2610(6) 0.0155(4) 0.3405(4) 0.0280(8) Uani d . 1 . .
C C21 0.3229(6) 0.2311(4) 0.0764(4) 0.0288(9) Uani d . 1 . .
C C22 0.5142(6) 0.2002(4) 0.0925(4) 0.0259(8) Uani d . 1 . .
C C23 0.6174(6) 0.1385(4) -0.0042(4) 0.0305(9) Uani d . 1 . .
H H23A 0.5724 0.1174 -0.0834 0.037 Uiso calc R 1 . .
C C24 0.7881(6) 0.1089(4) 0.0187(4) 0.0331(9) Uani d . 1 . .
H H24A 0.8581 0.0655 -0.0451 0.040 Uiso calc R 1 . .
C C25 0.8540(6) 0.1445(4) 0.1380(4) 0.0304(9) Uani d . 1 . .
H H25A 0.9681 0.1250 0.1556 0.036 Uiso calc R 1 . .
C C26 0.7457(6) 0.2100(4) 0.2303(4) 0.0263(8) Uani d . 1 . .
C C27 0.8038(6) 0.2583(4) 0.3617(4) 0.0304(9) Uani d . 1 . .
Co Co1 0.0000 0.5000 0.0000 0.02622(16) Uani d S 1 . .
O O1 -0.2898(5) 0.4621(4) -0.0162(3) 0.0439(8) Uani d D 1 . .
H H1A -0.359(6) 0.463(6) 0.039(3) 0.053 Uiso d D 1 . .
H H1B -0.356(6) 0.471(6) -0.069(4) 0.053 Uiso d D 1 . .
O O2 -0.0030(5) 0.5428(3) -0.1541(3) 0.0376(7) Uani d D 1 . .
H H2A -0.022(7) 0.478(3) -0.221(3) 0.045 Uiso d D 1 . .
H H2B -0.071(6) 0.596(4) -0.159(4) 0.045 Uiso d D 1 . .
O O3 -0.0090(5) 0.6937(3) 0.1035(3) 0.0387(8) Uani d D 1 . .
H H3A -0.077(6) 0.730(4) 0.074(5) 0.046 Uiso d D 1 . .
H H3B 0.066(6) 0.756(3) 0.153(4) 0.046 Uiso d D 1 . .
O O4 -0.0665(17) 0.3260(6) 0.6517(5) 0.146(4) Uani d D 1 . .
H H4A -0.077(19) 0.250(5) 0.652(10) 0.176 Uiso d D 1 . .
H H4B -0.058(19) 0.315(11) 0.579(3) 0.176 Uiso 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'
Co Co 0.3494 0.9721 '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
_geom_angle_publ_flag
O23 Bi1 O13 . . 93.19(12) ?
O23 Bi1 N2 . . 68.79(11) ?
O13 Bi1 N2 . . 73.57(12) ?
O23 Bi1 O11 . 2_666 79.71(12) ?
O13 Bi1 O11 . 2_666 156.24(11) ?
N2 Bi1 O11 . 2_666 82.74(11) ?
O23 Bi1 N1 . . 73.56(11) ?
O13 Bi1 N1 . . 67.02(11) ?
N2 Bi1 N1 . . 122.67(11) ?
O11 Bi1 N1 2_666 . 130.55(11) ?
O23 Bi1 O21 . . 134.27(10) ?
O13 Bi1 O21 . . 78.84(11) ?
N2 Bi1 O21 . . 65.75(11) ?
O11 Bi1 O21 2_666 . 89.88(11) ?
N1 Bi1 O21 . . 137.88(11) ?
O23 Bi1 O11 . . 72.66(11) ?
O13 Bi1 O11 . . 129.08(10) ?
N2 Bi1 O11 . . 136.25(11) ?
O11 Bi1 O11 2_666 . 70.63(11) ?
N1 Bi1 O11 . . 62.07(10) ?
O21 Bi1 O11 . . 144.46(10) ?
C16 N1 C12 . . 119.8(4) ?
C16 N1 Bi1 . . 116.0(3) ?
C12 N1 Bi1 . . 124.2(3) ?
C22 N2 C26 . . 120.9(4) ?
C22 N2 Bi1 . . 121.7(3) ?
C26 N2 Bi1 . . 116.9(3) ?
C11 O11 Bi1 . 2_666 126.3(3) ?
C11 O11 Bi1 . . 120.5(3) ?
Bi1 O11 Bi1 2_666 . 109.37(11) ?
C17 O13 Bi1 . . 124.3(3) ?
C21 O21 Bi1 . . 119.5(3) ?
C27 O23 Bi1 . . 122.6(3) ?
O12 C11 O11 . . 125.7(4) ?
O12 C11 C12 . . 118.9(4) ?
O11 C11 C12 . . 115.4(4) ?
N1 C12 C13 . . 121.1(4) ?
N1 C12 C11 . . 117.4(4) ?
C13 C12 C11 . . 121.4(4) ?
C14 C13 C12 . . 119.4(4) ?
C14 C13 H13A . . 120.3 ?
C12 C13 H13A . . 120.3 ?
C13 C14 C15 . . 119.3(4) ?
C13 C14 H14A . . 120.3 ?
C15 C14 H14A . . 120.3 ?
C16 C15 C14 . . 118.6(4) ?
C16 C15 H15A . . 120.7 ?
C14 C15 H15A . . 120.7 ?
N1 C16 C15 . . 121.7(4) ?
N1 C16 C17 . . 115.6(4) ?
C15 C16 C17 . . 122.7(4) ?
O14 C17 O13 . . 125.0(4) ?
O14 C17 C16 . . 118.3(4) ?
O13 C17 C16 . . 116.7(4) ?
O22 C21 O21 . . 127.0(4) ?
O22 C21 C22 . . 116.5(4) ?
O21 C21 C22 . . 116.5(4) ?
N2 C22 C23 . . 121.1(4) ?
N2 C22 C21 . . 115.9(4) ?
C23 C22 C21 . . 123.0(4) ?
C24 C23 C22 . . 119.1(4) ?
C24 C23 H23A . . 120.5 ?
C22 C23 H23A . . 120.5 ?
C23 C24 C25 . . 119.3(4) ?
C23 C24 H24A . . 120.4 ?
C25 C24 H24A . . 120.4 ?
C26 C25 C24 . . 118.5(4) ?
C26 C25 H25A . . 120.8 ?
C24 C25 H25A . . 120.8 ?
N2 C26 C25 . . 121.1(4) ?
N2 C26 C27 . . 115.1(4) ?
C25 C26 C27 . . 123.7(4) ?
O24 C27 O23 . . 124.1(4) ?
O24 C27 C26 . . 120.3(4) ?
O23 C27 C26 . . 115.6(4) ?
O3 Co1 O3 2_565 . 180.0(3) ?
O3 Co1 O2 2_565 2_565 88.90(14) ?
O3 Co1 O2 . 2_565 91.10(14) ?
O3 Co1 O2 2_565 . 91.10(14) ?
O3 Co1 O2 . . 88.90(14) ?
O2 Co1 O2 2_565 . 180.00(17) ?
O3 Co1 O1 2_565 2_565 90.42(16) ?
O3 Co1 O1 . 2_565 89.58(16) ?
O2 Co1 O1 2_565 2_565 89.79(15) ?
O2 Co1 O1 . 2_565 90.21(15) ?
O3 Co1 O1 2_565 . 89.58(16) ?
O3 Co1 O1 . . 90.42(16) ?
O2 Co1 O1 2_565 . 90.21(15) ?
O2 Co1 O1 . . 89.79(15) ?
O1 Co1 O1 2_565 . 180.0 ?
Co1 O1 H1A . . 126(4) ?
Co1 O1 H1B . . 124(3) ?
H1A O1 H1B . . 105.9(17) ?
Co1 O2 H2A . . 116(4) ?
Co1 O2 H2B . . 119(4) ?
H2A O2 H2B . . 105.6(17) ?
Co1 O3 H3A . . 115(3) ?
Co1 O3 H3B . . 135(3) ?
H3A O3 H3B . . 104.3(16) ?
H4A O4 H4B . . 105.0(17) ?
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 O23 . 2.269(3) ?
Bi1 O13 . 2.307(3) ?
Bi1 N2 . 2.372(3) ?
Bi1 O11 2_666 2.493(3) ?
Bi1 N1 . 2.494(3) ?
Bi1 O21 . 2.498(3) ?
Bi1 O11 . 2.682(3) ?
N1 C16 . 1.331(5) ?
N1 C12 . 1.338(5) ?
N2 C22 . 1.323(5) ?
N2 C26 . 1.337(5) ?
O11 C11 . 1.281(5) ?
O11 Bi1 2_666 2.493(3) ?
O12 C11 . 1.233(5) ?
O13 C17 . 1.272(5) ?
O14 C17 . 1.223(5) ?
O21 C21 . 1.256(5) ?
O22 C21 . 1.234(5) ?
O23 C27 . 1.285(5) ?
O24 C27 . 1.230(5) ?
C11 C12 . 1.507(6) ?
C12 C13 . 1.381(6) ?
C13 C14 . 1.367(7) ?
C13 H13A . 0.9300 ?
C14 C15 . 1.383(7) ?
C14 H14A . 0.9300 ?
C15 C16 . 1.382(6) ?
C15 H15A . 0.9300 ?
C16 C17 . 1.508(6) ?
C21 C22 . 1.508(6) ?
C22 C23 . 1.386(6) ?
C23 C24 . 1.380(7) ?
C23 H23A . 0.9300 ?
C24 C25 . 1.389(7) ?
C24 H24A . 0.9300 ?
C25 C26 . 1.387(6) ?
C25 H25A . 0.9300 ?
C26 C27 . 1.490(6) ?
Co1 O3 2_565 2.044(3) ?
Co1 O3 . 2.044(3) ?
Co1 O2 2_565 2.084(3) ?
Co1 O2 . 2.084(3) ?
Co1 O1 2_565 2.094(3) ?
Co1 O1 . 2.094(3) ?
O1 H1A . 0.836(10) ?
O1 H1B . 0.835(10) ?
O2 H2A . 0.836(10) ?
O2 H2B . 0.837(10) ?
O3 H3A . 0.839(10) ?
O3 H3B . 0.841(10) ?
O4 H4A . 0.840(10) ?
O4 H4B . 0.839(10) ?
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
O1 H1A O12 2_566 0.836(10) 2.04(2) 2.848(5) 163(6) yes
O1 H1B O12 1_454 0.835(10) 2.079(12) 2.913(5) 177(6) yes
O2 H2A O4 1_554 0.836(10) 1.778(14) 2.607(6) 171(6) yes
O2 H2B O21 2_565 0.837(10) 2.002(11) 2.839(5) 178(5) yes
O3 H3A O22 2_565 0.839(10) 1.807(17) 2.631(5) 167(6) yes
O3 H3B O14 1_565 0.841(10) 1.958(17) 2.785(5) 167(6) yes
O4 H4A O14 2_556 0.840(10) 2.11(6) 2.885(7) 153(12) yes
O4 H4B O24 1_455 0.839(10) 2.07(2) 2.898(7) 171(11) yes
