#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/80/2018022.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_2018022
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          '[Ni (H2 O)6] [Bi2 (C7 H4 N O4)4] , 2H2 O'
_chemical_formula_moiety         'H12 Ni1 O6 2+, C27 H16 Bi2 N4 O16 2-, 2H2 O'
_chemical_formula_sum            'C28 H28 Bi2 N4 Ni O24'
_chemical_formula_weight         1281.21
_chemical_name_systematic
;
hexaaquacobalt(II) bis(μ-pyridine-2,6-dicarboxylato)bis[(pyridine-2,6-
dicarboxylato)nickelate(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                112.96(3)
_cell_angle_beta                 90.79(3)
_cell_angle_gamma                97.33(3)
_cell_formula_units_Z            1
_cell_length_a                   7.2615(15)
_cell_length_b                   11.210(2)
_cell_length_c                   12.014(2)
_cell_measurement_reflns_used    8595
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.835
_cell_volume                     891.0(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 0.953
_diffrn_measured_fraction_theta_max 0.953
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0340
_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            10920
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    10.479
_exptl_absorpt_correction_T_max  0.3661
_exptl_absorpt_correction_T_min  0.2689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            light-green
_exptl_crystal_density_diffrn    2.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             610
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.055
_refine_diff_density_min         -0.846
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         4214
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0212
_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)+(0.0218P)²+0.3727P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0477
_refine_ls_wR_factor_ref         0.0502
_reflns_number_gt                3837
_reflns_number_total             4214
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sq3274.cif
_cod_data_source_block           II
_cod_original_cell_volume        891.0(3)
_cod_database_code               2018022
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 0.388113(17) 0.312794(11) 0.371459(11) 0.02065(5) Uani d . 1 . .
N N1 0.3443(4) 0.2100(3) 0.5218(3) 0.0220(6) Uani d . 1 . .
N N2 0.5790(4) 0.2347(3) 0.2063(3) 0.0203(6) Uani d . 1 . .
O O11 0.4418(4) 0.4700(2) 0.6081(2) 0.0299(6) Uani d . 1 . .
O O12 0.4719(4) 0.4843(3) 0.7984(2) 0.0341(6) Uani d . 1 . .
O O13 0.3067(4) 0.0883(2) 0.2805(2) 0.0316(6) Uani d . 1 . .
O O14 0.2033(5) -0.1015(3) 0.2917(3) 0.0442(8) Uani d . 1 . .
O O21 0.2411(3) 0.2857(2) 0.1712(2) 0.0269(5) Uani d . 1 . .
O O22 0.2625(4) 0.2032(3) -0.0288(3) 0.0465(8) Uani d . 1 . .
O O23 0.6780(4) 0.2988(3) 0.4358(2) 0.0311(6) Uani d . 1 . .
O O24 0.9667(4) 0.2579(3) 0.3959(3) 0.0431(7) Uani d . 1 . .
C C11 0.4356(5) 0.4221(3) 0.6886(3) 0.0232(7) Uani d . 1 . .
C C12 0.3764(5) 0.2756(3) 0.6416(3) 0.0231(7) Uani d . 1 . .
C C13 0.3529(6) 0.2119(4) 0.7198(3) 0.0319(8) Uani d . 1 . .
H H13A 0.3797 0.2577 0.8028 0.038 Uiso calc R 1 . .
C C14 0.2898(7) 0.0810(4) 0.6733(4) 0.0428(11) Uani d . 1 . .
H H14A 0.2699 0.0373 0.7248 0.051 Uiso calc R 1 . .
C C15 0.2553(6) 0.0131(4) 0.5498(4) 0.0380(10) Uani d . 1 . .
H H15A 0.2125 -0.0763 0.5171 0.046 Uiso calc R 1 . .
C C16 0.2860(5) 0.0812(3) 0.4756(3) 0.0248(7) Uani d . 1 . .
C C17 0.2612(5) 0.0158(4) 0.3397(3) 0.0278(8) Uani d . 1 . .
C C21 0.3233(5) 0.2324(4) 0.0757(3) 0.0257(7) Uani d . 1 . .
C C22 0.5159(5) 0.2006(3) 0.0925(3) 0.0221(7) Uani d . 1 . .
C C23 0.6191(6) 0.1392(4) -0.0034(3) 0.0293(8) Uani d . 1 . .
H H23A 0.5747 0.1186 -0.0827 0.035 Uiso calc R 1 . .
C C24 0.7902(5) 0.1090(4) 0.0206(3) 0.0312(8) Uani d . 1 . .
H H24A 0.8606 0.0651 -0.0427 0.037 Uiso calc R 1 . .
C C25 0.8557(5) 0.1447(4) 0.1398(4) 0.0285(8) Uani d . 1 . .
H H25A 0.9699 0.1247 0.1577 0.034 Uiso calc R 1 . .
C C26 0.7483(5) 0.2104(3) 0.2310(3) 0.0220(7) Uani d . 1 . .
C C27 0.8054(5) 0.2587(4) 0.3627(3) 0.0267(8) Uani d . 1 . .
Ni Ni1 0.0000 0.5000 0.0000 0.02368(13) Uani d S 1 . .
O O1 -0.2866(4) 0.4586(3) -0.0175(3) 0.0400(7) Uani d D 1 . .
H H1A -0.345(5) 0.467(5) 0.043(2) 0.048 Uiso d D 1 . .
H H1B -0.358(5) 0.470(5) -0.066(3) 0.048 Uiso d D 1 . .
O O2 0.0047(4) 0.5436(3) -0.1505(2) 0.0341(6) Uani d D 1 . .
H H2A -0.030(5) 0.476(2) -0.213(3) 0.041 Uiso d D 1 . .
H H2B -0.072(5) 0.594(3) -0.149(4) 0.041 Uiso d D 1 . .
O O3 -0.0126(4) 0.6901(3) 0.1053(3) 0.0363(7) Uani d D 1 . .
H H3A -0.083(4) 0.731(3) 0.082(4) 0.044 Uiso d D 1 . .
H H3B 0.079(4) 0.745(3) 0.142(4) 0.044 Uiso d D 1 . .
O O4 -0.0812(13) 0.3289(4) 0.6558(4) 0.144(3) Uani d D 1 . .
H H4A -0.080(15) 0.251(3) 0.646(8) 0.173 Uiso d D 1 . .
H H4B -0.067(14) 0.332(8) 0.588(4) 0.173 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'
Ni Ni 0.3393 1.1124 '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 . . 93.28(10) ?
O23 Bi1 N2 . . 68.68(9) ?
O13 Bi1 N2 . . 72.91(10) ?
O23 Bi1 N1 . . 73.46(10) ?
O13 Bi1 N1 . . 67.39(9) ?
N2 Bi1 N1 . . 122.22(9) ?
O23 Bi1 O11 . 2_666 79.49(10) ?
O13 Bi1 O11 . 2_666 155.11(9) ?
N2 Bi1 O11 . 2_666 82.30(9) ?
N1 Bi1 O11 . 2_666 131.06(9) ?
O23 Bi1 O21 . . 134.06(9) ?
O13 Bi1 O21 . . 78.75(9) ?
N2 Bi1 O21 . . 65.72(9) ?
N1 Bi1 O21 . . 138.26(9) ?
O11 Bi1 O21 2_666 . 89.20(9) ?
O23 Bi1 O11 . . 72.58(9) ?
O13 Bi1 O11 . . 129.42(9) ?
N2 Bi1 O11 . . 136.28(9) ?
N1 Bi1 O11 . . 62.04(8) ?
O11 Bi1 O11 2_666 . 71.33(9) ?
O21 Bi1 O11 . . 144.48(8) ?
C16 N1 C12 . . 120.1(3) ?
C16 N1 Bi1 . . 115.8(2) ?
C12 N1 Bi1 . . 124.1(2) ?
C22 N2 C26 . . 120.2(3) ?
C22 N2 Bi1 . . 122.2(2) ?
C26 N2 Bi1 . . 117.1(2) ?
C11 O11 Bi1 . 2_666 126.7(2) ?
C11 O11 Bi1 . . 120.7(2) ?
Bi1 O11 Bi1 2_666 . 108.67(9) ?
C17 O13 Bi1 . . 123.6(2) ?
C21 O21 Bi1 . . 119.2(2) ?
C27 O23 Bi1 . . 122.6(2) ?
O12 C11 O11 . . 125.9(3) ?
O12 C11 C12 . . 118.8(3) ?
O11 C11 C12 . . 115.3(3) ?
N1 C12 C13 . . 121.1(3) ?
N1 C12 C11 . . 117.6(3) ?
C13 C12 C11 . . 121.3(3) ?
C14 C13 C12 . . 118.9(4) ?
C14 C13 H13A . . 120.5 ?
C12 C13 H13A . . 120.5 ?
C13 C14 C15 . . 120.1(4) ?
C13 C14 H14A . . 119.9 ?
C15 C14 H14A . . 119.9 ?
C14 C15 C16 . . 118.4(4) ?
C14 C15 H15A . . 120.8 ?
C16 C15 H15A . . 120.8 ?
N1 C16 C15 . . 121.2(3) ?
N1 C16 C17 . . 115.9(3) ?
C15 C16 C17 . . 122.8(3) ?
O14 C17 O13 . . 123.9(4) ?
O14 C17 C16 . . 119.2(3) ?
O13 C17 C16 . . 116.9(3) ?
O22 C21 O21 . . 126.7(3) ?
O22 C21 C22 . . 116.8(3) ?
O21 C21 C22 . . 116.5(3) ?
N2 C22 C23 . . 121.7(3) ?
N2 C22 C21 . . 115.5(3) ?
C23 C22 C21 . . 122.8(3) ?
C22 C23 C24 . . 118.6(3) ?
C22 C23 H23A . . 120.7 ?
C24 C23 H23A . . 120.7 ?
C23 C24 C25 . . 119.5(3) ?
C23 C24 H24A . . 120.3 ?
C25 C24 H24A . . 120.3 ?
C26 C25 C24 . . 118.6(3) ?
C26 C25 H25A . . 120.7 ?
C24 C25 H25A . . 120.7 ?
N2 C26 C25 . . 121.3(3) ?
N2 C26 C27 . . 114.6(3) ?
C25 C26 C27 . . 124.1(3) ?
O24 C27 O23 . . 123.8(3) ?
O24 C27 C26 . . 120.1(3) ?
O23 C27 C26 . . 116.1(3) ?
O3 Ni1 O3 2_565 . 180.0(2) ?
O3 Ni1 O2 2_565 2_565 89.91(12) ?
O3 Ni1 O2 . 2_565 90.09(12) ?
O3 Ni1 O2 2_565 . 90.09(12) ?
O3 Ni1 O2 . . 89.91(12) ?
O2 Ni1 O2 2_565 . 180.00(14) ?
O3 Ni1 O1 2_565 . 89.10(13) ?
O3 Ni1 O1 . . 90.90(13) ?
O2 Ni1 O1 2_565 . 88.32(12) ?
O2 Ni1 O1 . . 91.68(12) ?
O3 Ni1 O1 2_565 2_565 90.90(13) ?
O3 Ni1 O1 . 2_565 89.10(13) ?
O2 Ni1 O1 2_565 2_565 91.68(12) ?
O2 Ni1 O1 . 2_565 88.32(12) ?
O1 Ni1 O1 . 2_565 180.0 ?
Ni1 O1 H1A . . 120(3) ?
Ni1 O1 H1B . . 127(3) ?
H1A O1 H1B . . 106.1(16) ?
Ni1 O2 H2A . . 110(3) ?
Ni1 O2 H2B . . 112(3) ?
H2A O2 H2B . . 104.6(16) ?
Ni1 O3 H3A . . 119(3) ?
Ni1 O3 H3B . . 125(3) ?
H3A O3 H3B . . 105.1(16) ?
H4A O4 H4B . . 105.8(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 . 2.277(3) ?
Bi1 O13 . 2.310(3) ?
Bi1 N2 . 2.378(3) ?
Bi1 N1 . 2.497(3) ?
Bi1 O11 2_666 2.504(3) ?
Bi1 O21 . 2.510(3) ?
Bi1 O11 . 2.688(3) ?
N1 C16 . 1.337(4) ?
N1 C12 . 1.337(4) ?
N2 C22 . 1.325(4) ?
N2 C26 . 1.346(4) ?
O11 C11 . 1.275(4) ?
O11 Bi1 2_666 2.504(3) ?
O12 C11 . 1.234(4) ?
O13 C17 . 1.289(4) ?
O14 C17 . 1.225(4) ?
O21 C21 . 1.266(4) ?
O22 C21 . 1.227(4) ?
O23 C27 . 1.285(4) ?
O24 C27 . 1.235(4) ?
C11 C12 . 1.514(5) ?
C12 C13 . 1.386(5) ?
C13 C14 . 1.363(6) ?
C13 H13A . 0.9300 ?
C14 C15 . 1.380(6) ?
C14 H14A . 0.9300 ?
C15 C16 . 1.385(5) ?
C15 H15A . 0.9300 ?
C16 C17 . 1.503(5) ?
C21 C22 . 1.517(5) ?
C22 C23 . 1.379(5) ?
C23 C24 . 1.384(6) ?
C23 H23A . 0.9300 ?
C24 C25 . 1.386(5) ?
C24 H24A . 0.9300 ?
C25 C26 . 1.375(5) ?
C25 H25A . 0.9300 ?
C26 C27 . 1.492(5) ?
Ni1 O3 2_565 2.024(3) ?
Ni1 O3 . 2.024(3) ?
Ni1 O2 2_565 2.049(3) ?
Ni1 O2 . 2.049(3) ?
Ni1 O1 . 2.063(3) ?
Ni1 O1 2_565 2.063(3) ?
O1 H1A . 0.832(10) ?
O1 H1B . 0.835(10) ?
O2 H2A . 0.839(10) ?
O2 H2B . 0.838(10) ?
O3 H3A . 0.839(10) ?
O3 H3B . 0.835(10) ?
O4 H4A . 0.835(10) ?
O4 H4B . 0.837(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 0.832(10) 2.030(13) 2.856(4) 172(5) yes
O1 H1B O12 1_454 0.835(10) 2.095(11) 2.927(4) 174(4) yes
O2 H2A O4 1_554 0.839(10) 1.771(11) 2.608(5) 175(4) yes
O2 H2B O21 2_565 0.838(10) 2.023(13) 2.852(4) 170(4) yes
O3 H3A O22 2_565 0.839(10) 1.803(11) 2.634(4) 170(4) yes
O3 H3B O14 1_565 0.835(10) 2.04(3) 2.796(4) 151(4) yes
O4 H4A O14 2_556 0.835(10) 2.19(6) 2.895(6) 142(8) yes
O4 H4B O24 1_455 0.837(10) 2.15(4) 2.944(6) 157(8) yes
