#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/99/2219954.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_2219954
loop_
_publ_author_name
'Nettleman, Joseph H.'
'LaDuca, Robert L.'
_publ_section_title
;catena-Poly[[[tetraaquacobalt(II)]-μ-4,4'-bipyridine-κ²N:N']
 bis(perchlorate) 4,4'-bipyridine disolvate dihydrate]
;
_journal_coeditor_code           NG2505
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1485
_journal_paper_doi               10.1107/S1600536808035125
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac
'[Co (C10 H8 N2) (H2 O)4] (Cl O4)2, 2C10 H8 N2, 2H2 O'
_chemical_formula_moiety
'C10 H16 Co N2 O4 2+, 2(Cl O4-), 2(C10 H8 N2), 2(H2 O)'
_chemical_formula_sum            'C30 H36 Cl2 Co N6 O14'
_chemical_formula_weight         834.48
_chemical_name_systematic
;
catena-Poly[[[tetraaquacobalt(II)]-μ-4,4'-bipyridine-κ²N:N']
perchlorate 4,4'-bipyridine disolvate 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           SHELXL-97
_cell_angle_alpha                64.290(2)
_cell_angle_beta                 71.747(2)
_cell_angle_gamma                66.848(2)
_cell_formula_units_Z            1
_cell_length_a                   8.9590(17)
_cell_length_b                   10.846(2)
_cell_length_c                   11.433(2)
_cell_measurement_reflns_used    10254
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.01
_cell_volume                     906.6(3)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT-Plus  (Bruker, 2003)'
_computing_molecular_graphics    'Crystal Maker (Palmer, 2007)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'Bruker SMART 1K'
_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  0.0178
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_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            10254
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  0.8453
_exptl_absorpt_correction_T_min  0.7928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             431
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.321
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4087
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0302
_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)+(0.0438P)²+0.4101P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0854
_reflns_number_gt                3754
_reflns_number_total             4087
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng2505.cif
_cod_data_source_block           I
_cod_database_code               2219954
_cod_database_fobs_code          2219954
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
Co Co1 0.5000 0.0000 0.5000 0.02019(9) Uani d S 1
Cl Cl1 0.08313(6) 0.68822(5) 0.28417(4) 0.03844(12) Uani d . 1
O O1 0.49177(16) 0.21628(12) 0.41627(11) 0.0331(3) Uani d D 1
H H1A 0.432(2) 0.272(2) 0.4590(19) 0.040 Uiso d D 1
H H1B 0.527(2) 0.269(2) 0.3396(16) 0.040 Uiso d D 1
O O1W 0.31208(19) 0.40133(17) 0.54939(15) 0.0471(3) Uani d D 1
H H1WA 0.233(3) 0.366(2) 0.602(2) 0.057 Uiso d D 1
H H1WB 0.258(3) 0.4859(19) 0.499(2) 0.057 Uiso d D 1
O O2 0.75905(14) -0.06554(13) 0.46036(11) 0.0291(2) Uani d D 1
H H2A 0.818(2) -0.0077(19) 0.4057(18) 0.035 Uiso d D 1
H H2B 0.809(2) -0.1404(17) 0.4406(19) 0.035 Uiso d D 1
O O3 -0.0888(2) 0.76945(18) 0.28167(18) 0.0592(4) Uani d . 1
O O4 0.1008(2) 0.53921(16) 0.32135(15) 0.0576(4) Uani d . 1
O O5 0.1756(2) 0.73950(19) 0.15629(15) 0.0586(4) Uani d . 1
O O6 0.1383(3) 0.7065(2) 0.37918(17) 0.0661(5) Uani d . 1
N N1 0.49875(15) -0.00436(13) 0.31409(11) 0.0222(2) Uani d . 1
N N6 -0.05017(19) 0.09941(17) 0.28287(17) 0.0413(4) Uani d . 1
N N7 0.3813(2) 0.59027(15) -0.19049(14) 0.0368(3) Uani d . 1
C C1 0.5839(2) 0.06703(17) 0.20323(14) 0.0269(3) Uani d . 1
H H1 0.6438 0.1163 0.2098 0.032 Uiso calc R 1
C C2 0.5878(2) 0.07151(17) 0.07951(14) 0.0263(3) Uani d . 1
H H2 0.6488 0.1230 0.0057 0.032 Uiso calc R 1
C C3 0.49982(17) -0.00143(15) 0.06583(13) 0.0195(3) Uani d . 1
C C4 0.41216(18) -0.07678(16) 0.18123(14) 0.0240(3) Uani d . 1
H H4 0.3528 -0.1284 0.1777 0.029 Uiso calc R 1
C C5 0.41367(19) -0.07458(16) 0.30132(14) 0.0246(3) Uani d . 1
H H5 0.3527 -0.1242 0.3767 0.030 Uiso calc R 1
C C11 -0.0014(3) 0.1789(2) 0.3167(2) 0.0486(5) Uani d . 1
H H11 -0.0296 0.1723 0.4043 0.058 Uiso calc R 1
C C12 0.0890(3) 0.2709(2) 0.22857(18) 0.0462(5) Uani d . 1
H H12 0.1211 0.3231 0.2576 0.055 Uiso calc R 1
C C13 0.13149(19) 0.28494(16) 0.09666(16) 0.0292(3) Uani d . 1
C C14 0.0826(2) 0.20049(19) 0.06118(19) 0.0358(4) Uani d . 1
H H14 0.1089 0.2049 -0.0257 0.043 Uiso calc R 1
C C15 -0.0056(2) 0.1098(2) 0.1566(2) 0.0413(4) Uani d . 1
H H15 -0.0355 0.0530 0.1315 0.050 Uiso calc R 1
C C16 0.3327(3) 0.5801(2) -0.06572(18) 0.0414(4) Uani d . 1
H H16 0.3518 0.6430 -0.0410 0.050 Uiso calc R 1
C C17 0.2551(3) 0.4816(2) 0.03043(17) 0.0404(4) Uani d . 1
H H17 0.2253 0.4787 0.1170 0.048 Uiso calc R 1
C C18 0.22204(19) 0.38758(16) -0.00284(15) 0.0279(3) Uani d . 1
C C19 0.2767(3) 0.3953(2) -0.13273(19) 0.0515(5) Uani d . 1
H H19 0.2608 0.3330 -0.1603 0.062 Uiso calc R 1
C C20 0.3555(3) 0.4965(2) -0.22154(19) 0.0544(6) Uani d . 1
H H20 0.3924 0.4988 -0.3079 0.065 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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
O1 Co1 O1 2_656 . 180.0000(10)
O1 Co1 O2 2_656 2_656 91.24(5)
O1 Co1 O2 . 2_656 88.76(5)
O1 Co1 O2 2_656 . 88.76(5)
O1 Co1 O2 . . 91.24(5)
O2 Co1 O2 2_656 . 180.0
O1 Co1 N1 2_656 . 87.77(5)
O1 Co1 N1 . . 92.23(5)
O2 Co1 N1 2_656 . 90.66(4)
O2 Co1 N1 . . 89.34(4)
O1 Co1 N1 2_656 2_656 92.23(5)
O1 Co1 N1 . 2_656 87.77(5)
O2 Co1 N1 2_656 2_656 89.34(4)
O2 Co1 N1 . 2_656 90.66(4)
N1 Co1 N1 . 2_656 180.0
O5 Cl1 O4 . . 110.45(9)
O5 Cl1 O6 . . 110.12(11)
O4 Cl1 O6 . . 109.46(11)
O5 Cl1 O3 . . 108.74(11)
O4 Cl1 O3 . . 108.86(11)
O6 Cl1 O3 . . 109.19(11)
Co1 O1 H1A . . 119.4(14)
Co1 O1 H1B . . 133.1(14)
H1A O1 H1B . . 106.9(18)
H1WA O1W H1WB . . 102(2)
Co1 O2 H2A . . 123.8(13)
Co1 O2 H2B . . 118.8(13)
H2A O2 H2B . . 101.8(18)
C1 N1 C5 . . 116.71(12)
C1 N1 Co1 . . 119.99(9)
C5 N1 Co1 . . 123.29(9)
C11 N6 C15 . . 116.74(16)
C16 N7 C20 . . 116.24(15)
N1 C1 C2 . . 123.68(13)
N1 C1 H1 . . 118.2
C2 C1 H1 . . 118.2
C1 C2 C3 . . 119.79(13)
C1 C2 H2 . . 120.1
C3 C2 H2 . . 120.1
C4 C3 C2 . . 116.62(12)
C4 C3 C3 . 2_655 121.98(15)
C2 C3 C3 . 2_655 121.39(15)
C5 C4 C3 . . 119.88(13)
C5 C4 H4 . . 120.1
C3 C4 H4 . . 120.1
N1 C5 C4 . . 123.30(13)
N1 C5 H5 . . 118.3
C4 C5 H5 . . 118.3
N6 C11 C12 . . 123.61(19)
N6 C11 H11 . . 118.2
C12 C11 H11 . . 118.2
C11 C12 C13 . . 119.77(18)
C11 C12 H12 . . 120.1
C13 C12 H12 . . 120.1
C12 C13 C14 . . 116.80(16)
C12 C13 C18 . . 121.64(16)
C14 C13 C18 . . 121.55(15)
C15 C14 C13 . . 119.38(17)
C15 C14 H14 . . 120.3
C13 C14 H14 . . 120.3
N6 C15 C14 . . 123.67(18)
N6 C15 H15 . . 118.2
C14 C15 H15 . . 118.2
N7 C16 C17 . . 124.13(17)
N7 C16 H16 . . 117.9
C17 C16 H16 . . 117.9
C18 C17 C16 . . 119.71(16)
C18 C17 H17 . . 120.1
C16 C17 H17 . . 120.1
C17 C18 C19 . . 116.31(15)
C17 C18 C13 . . 121.17(15)
C19 C18 C13 . . 122.51(16)
C18 C19 C20 . . 119.67(18)
C18 C19 H19 . . 120.2
C20 C19 H19 . . 120.2
N7 C20 C19 . . 123.85(18)
N7 C20 H20 . . 118.1
C19 C20 H20 . . 118.1
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co1 O1 2_656 2.0938(12)
Co1 O1 . 2.0938(12)
Co1 O2 2_656 2.1024(12)
Co1 O2 . 2.1024(12)
Co1 N1 . 2.1500(12)
Co1 N1 2_656 2.1500(12)
Cl1 O5 . 1.4251(15)
Cl1 O4 . 1.4361(15)
Cl1 O6 . 1.4365(16)
Cl1 O3 . 1.4450(17)
O1 H1A . 0.856(15)
O1 H1B . 0.852(15)
O1W H1WA . 0.868(16)
O1W H1WB . 0.881(16)
O2 H2A . 0.883(15)
O2 H2B . 0.849(15)
N1 C1 . 1.3399(18)
N1 C5 . 1.3435(18)
N6 C11 . 1.333(3)
N6 C15 . 1.337(3)
N7 C16 . 1.322(2)
N7 C20 . 1.328(3)
C1 C2 . 1.384(2)
C1 H1 . 0.9300
C2 C3 . 1.3950(19)
C2 H2 . 0.9300
C3 C4 . 1.3948(19)
C3 C3 2_655 1.491(3)
C4 C5 . 1.3878(19)
C4 H4 . 0.9300
C5 H5 . 0.9300
C11 C12 . 1.385(3)
C11 H11 . 0.9300
C12 C13 . 1.389(3)
C12 H12 . 0.9300
C13 C14 . 1.395(2)
C13 C18 . 1.492(2)
C14 C15 . 1.387(3)
C14 H14 . 0.9300
C15 H15 . 0.9300
C16 C17 . 1.385(2)
C16 H16 . 0.9300
C17 C18 . 1.384(2)
C17 H17 . 0.9300
C18 C19 . 1.386(3)
C19 C20 . 1.388(3)
C19 H19 . 0.9300
C20 H20 . 0.9300
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 O1W . 0.856(15) 1.886(16) 2.7406(19) 176(2) y
O1 H1B N7 2_665 0.852(15) 1.943(16) 2.7744(18) 165(2) y
O1W H1WA O3 2_566 0.868(16) 2.079(17) 2.924(2) 164(2) y
O1W H1WB O6 . 0.881(16) 2.192(16) 3.070(3) 174(2) y
O2 H2A N6 1_655 0.883(15) 1.826(15) 2.7058(19) 174.1(19) y
O2 H2B O3 1_645 0.849(15) 2.212(17) 2.957(2) 146.5(18) y
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
O1 Co1 N1 C1 2_656 . -141.42(12)
O1 Co1 N1 C1 . . 38.58(12)
O2 Co1 N1 C1 2_656 . 127.37(12)
O2 Co1 N1 C1 . . -52.63(12)
O1 Co1 N1 C5 2_656 . 39.55(12)
O1 Co1 N1 C5 . . -140.45(12)
O2 Co1 N1 C5 2_656 . -51.66(12)
O2 Co1 N1 C5 . . 128.34(12)
C5 N1 C1 C2 . . 0.1(2)
Co1 N1 C1 C2 . . -179.04(13)
N1 C1 C2 C3 . . -0.2(3)
C1 C2 C3 C4 . . -0.4(2)
C1 C2 C3 C3 . 2_655 179.68(16)
C2 C3 C4 C5 . . 1.0(2)
C3 C3 C4 C5 2_655 . -179.08(16)
C1 N1 C5 C4 . . 0.6(2)
Co1 N1 C5 C4 . . 179.65(11)
C3 C4 C5 N1 . . -1.1(2)
C15 N6 C11 C12 . . 0.9(3)
N6 C11 C12 C13 . . 0.8(4)
C11 C12 C13 C14 . . -1.6(3)
C11 C12 C13 C18 . . 177.17(18)
C12 C13 C14 C15 . . 0.7(3)
C18 C13 C14 C15 . . -178.08(16)
C11 N6 C15 C14 . . -1.9(3)
C13 C14 C15 N6 . . 1.1(3)
C20 N7 C16 C17 . . -1.5(3)
N7 C16 C17 C18 . . -1.0(3)
C16 C17 C18 C19 . . 2.6(3)
C16 C17 C18 C13 . . -177.01(17)
C12 C13 C18 C17 . . -5.5(3)
C14 C13 C18 C17 . . 173.20(17)
C12 C13 C18 C19 . . 174.9(2)
C14 C13 C18 C19 . . -6.4(3)
C17 C18 C19 C20 . . -1.8(3)
C13 C18 C19 C20 . . 177.9(2)
C16 N7 C20 C19 . . 2.5(4)
C18 C19 C20 N7 . . -0.8(4)
