#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/16/2221604.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_2221604
loop_
_publ_author_name
'Wang, Hai-Dong'
'Li, Min-Min'
'He, Hong-Yin'
_publ_section_title
Poly[di-μ₂-acetato-diaquabis(2,2'-bipyridine)bis(μ₃-5-nitroisophthalato)tricobalt(II)]
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m510
_journal_paper_doi               10.1107/S1600536809012562
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac
'[Co3 (C8 H3 N O6)2 (C2 H3 O2)2 (C10 H8 N2)2 (H2 O)2]'
_chemical_formula_moiety         'C40 H32 Co3 N6 O18'
_chemical_formula_sum            'C40 H32 Co3 N6 O18'
_chemical_formula_weight         1061.51
_chemical_name_systematic
;
Poly[di-μ₂-acetato-diaquabis(2,2'-bipyridine)bis(μ₃-5-\
nitroisophthalato)tricobalt(II)]
;
_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                81.1960(10)
_cell_angle_beta                 67.6850(10)
_cell_angle_gamma                69.4720(10)
_cell_formula_units_Z            1
_cell_length_a                   10.00840(10)
_cell_length_b                   10.07810(10)
_cell_length_c                   11.39410(10)
_cell_measurement_reflns_used    10424
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      1.94
_cell_volume                     995.429(19)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART 1K CCD'
_diffrn_measurement_method       phi/omega
_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  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10424
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    1.327
_exptl_absorpt_correction_T_max  0.8832
_exptl_absorpt_correction_T_min  0.7241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             539
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.452
_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     310
_refine_ls_number_reflns         3679
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0299
_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)+(0.0358P)²+1.0580P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0773
_reflns_number_gt                3296
_reflns_number_total             3679
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt2923.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        995.430(17)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2221604
_cod_database_fobs_code          2221604
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
Co Co1 0.0000 1.0000 0.5000 0.02056(11) Uani d S 1 . .
Co Co2 0.29863(3) 0.66172(3) 0.34001(3) 0.02348(10) Uani d . 1 . .
N N1 0.5014(2) 0.4947(2) 0.26205(19) 0.0264(4) Uani d . 1 . .
N N2 0.2395(2) 0.5533(2) 0.23098(19) 0.0271(4) Uani d . 1 . .
C C6 0.3533(3) 0.4463(2) 0.1610(2) 0.0259(5) Uani d . 1 . .
O O1 0.38924(18) 0.74188(17) 0.43457(16) 0.0283(4) Uani d . 1 . .
O O9 0.10814(18) 0.86327(17) 0.34394(15) 0.0263(4) Uani d . 1 . .
C C11 0.5544(3) 0.8074(2) 0.5603(2) 0.0218(5) Uani d . 1 . .
H H11A 0.6088 0.7353 0.5017 0.026 Uiso calc R 1 . .
C C17 0.3124(3) 0.8272(2) 0.5243(2) 0.0233(5) Uani d . 1 . .
C C16 0.3980(3) 0.8686(2) 0.5891(2) 0.0219(5) Uani d . 1 . .
C C19 0.8024(3) 0.7950(3) 0.5801(2) 0.0269(5) Uani d . 1 . .
C C12 0.6310(3) 0.8526(2) 0.6180(2) 0.0233(5) Uani d . 1 . .
O O3 0.8695(2) 0.67757(19) 0.5289(2) 0.0414(5) Uani d . 1 . .
C C5 0.5033(3) 0.4180(2) 0.1738(2) 0.0256(5) Uani d . 1 . .
C C4 0.6363(3) 0.3199(3) 0.1018(2) 0.0337(6) Uani d . 1 . .
H H4A 0.6361 0.2703 0.0395 0.040 Uiso calc R 1 . .
C C14 0.3935(3) 1.0141(2) 0.7364(2) 0.0273(5) Uani d . 1 . .
C C13 0.5491(3) 0.9578(3) 0.7079(2) 0.0272(5) Uani d . 1 . .
H H13A 0.5977 0.9894 0.7478 0.033 Uiso calc R 1 . .
C C15 0.3160(3) 0.9740(2) 0.6786(2) 0.0262(5) Uani d . 1 . .
H H15A 0.2114 1.0163 0.6989 0.031 Uiso calc R 1 . .
C C9 0.0689(3) 0.5133(3) 0.1519(3) 0.0382(6) Uani d . 1 . .
H H9A -0.0288 0.5389 0.1495 0.046 Uiso calc R 1 . .
C C7 0.3293(3) 0.3687(3) 0.0849(3) 0.0352(6) Uani d . 1 . .
H H7A 0.4092 0.2951 0.0369 0.042 Uiso calc R 1 . .
C C10 0.1008(3) 0.5858(3) 0.2260(3) 0.0328(6) Uani d . 1 . .
H H10A 0.0225 0.6601 0.2742 0.039 Uiso calc R 1 . .
C C1 0.6309(3) 0.4698(3) 0.2832(3) 0.0327(6) Uani d . 1 . .
H H1A 0.6295 0.5217 0.3447 0.039 Uiso calc R 1 . .
C C8 0.1844(3) 0.4028(3) 0.0818(3) 0.0406(7) Uani d . 1 . .
H H8A 0.1652 0.3512 0.0324 0.049 Uiso calc R 1 . .
C C2 0.7661(3) 0.3707(3) 0.2180(3) 0.0379(6) Uani d . 1 . .
H H2A 0.8533 0.3539 0.2369 0.046 Uiso calc R 1 . .
N N3 0.3069(3) 1.1250(3) 0.8321(2) 0.0462(6) Uani d . 1 . .
C C3 0.7690(3) 0.2970(3) 0.1241(3) 0.0392(6) Uani d . 1 . .
H H3A 0.8598 0.2323 0.0761 0.047 Uiso calc R 1 . .
O O6 0.1710(3) 1.1769(3) 0.8577(3) 0.0776(9) Uani d . 1 . .
O O2 0.17072(18) 0.88101(19) 0.56665(16) 0.0318(4) Uani d . 1 . .
O O4 0.8652(2) 0.8704(2) 0.60355(17) 0.0369(4) Uani d . 1 . .
O O5 0.3732(3) 1.1514(4) 0.8890(3) 0.1161(15) Uani d . 1 . .
O O1W 0.17349(19) 0.56964(19) 0.50084(18) 0.0318(4) Uani d D 1 . .
H H1WA 0.0831(15) 0.620(2) 0.523(3) 0.048 Uiso d D 1 . .
H H1WB 0.180(3) 0.4895(15) 0.486(3) 0.048 Uiso d D 1 . .
O O8 0.31763(19) 0.80788(18) 0.17845(16) 0.0334(4) Uani d . 1 . .
C C32 0.1871(3) 0.8911(2) 0.2305(2) 0.0263(5) Uani d . 1 . .
C C33 0.1213(4) 1.0190(3) 0.1602(3) 0.0468(7) Uani d . 1 . .
H H33A 0.1949 1.0239 0.0772 0.070 Uiso calc R 1 . .
H H33B 0.0952 1.1025 0.2056 0.070 Uiso calc R 1 . .
H H33C 0.0314 1.0129 0.1524 0.070 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'
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
O2 Co1 O2 . 2_576 180.0 ?
O2 Co1 O9 . 2_576 92.58(6) ?
O2 Co1 O9 2_576 2_576 87.42(6) ?
O2 Co1 O9 . . 87.42(6) ?
O2 Co1 O9 2_576 . 92.58(6) ?
O9 Co1 O9 2_576 . 180.0000(10) ?
O2 Co1 O4 . 1_455 90.67(7) ?
O2 Co1 O4 2_576 1_455 89.33(7) ?
O9 Co1 O4 2_576 1_455 88.72(7) ?
O9 Co1 O4 . 1_455 91.28(7) ?
O2 Co1 O4 . 2_676 89.33(7) ?
O2 Co1 O4 2_576 2_676 90.67(7) ?
O9 Co1 O4 2_576 2_676 91.28(7) ?
O9 Co1 O4 . 2_676 88.72(7) ?
O4 Co1 O4 1_455 2_676 180.0 ?
O1 Co2 O1W . . 94.98(7) ?
O1 Co2 N1 . . 94.01(7) ?
O1W Co2 N1 . . 103.72(7) ?
O1 Co2 N2 . . 170.78(7) ?
O1W Co2 N2 . . 87.41(7) ?
N1 Co2 N2 . . 76.77(7) ?
O1 Co2 O8 . . 98.32(7) ?
O1W Co2 O8 . . 152.53(7) ?
N1 Co2 O8 . . 99.22(7) ?
N2 Co2 O8 . . 83.29(7) ?
O1 Co2 O9 . . 94.50(6) ?
O1W Co2 O9 . . 95.80(7) ?
N1 Co2 O9 . . 157.91(7) ?
N2 Co2 O9 . . 94.12(7) ?
O8 Co2 O9 . . 59.37(6) ?
C1 N1 C5 . . 118.4(2) ?
C1 N1 Co2 . . 124.99(16) ?
C5 N1 Co2 . . 116.21(15) ?
C10 N2 C6 . . 119.0(2) ?
C10 N2 Co2 . . 124.78(16) ?
C6 N2 Co2 . . 116.22(15) ?
N2 C6 C7 . . 121.6(2) ?
N2 C6 C5 . . 114.8(2) ?
C7 C6 C5 . . 123.6(2) ?
C17 O1 Co2 . . 124.66(14) ?
C32 O9 Co1 . . 126.76(14) ?
C32 O9 Co2 . . 88.61(13) ?
Co1 O9 Co2 . . 121.97(8) ?
C16 C11 C12 . . 121.0(2) ?
C16 C11 H11A . . 119.5 ?
C12 C11 H11A . . 119.5 ?
O2 C17 O1 . . 126.4(2) ?
O2 C17 C16 . . 116.0(2) ?
O1 C17 C16 . . 117.6(2) ?
C15 C16 C11 . . 119.6(2) ?
C15 C16 C17 . . 117.9(2) ?
C11 C16 C17 . . 122.5(2) ?
O3 C19 O4 . . 125.4(2) ?
O3 C19 C12 . . 118.0(2) ?
O4 C19 C12 . . 116.6(2) ?
C13 C12 C11 . . 119.5(2) ?
C13 C12 C19 . . 119.0(2) ?
C11 C12 C19 . . 121.4(2) ?
N1 C5 C4 . . 121.7(2) ?
N1 C5 C6 . . 115.1(2) ?
C4 C5 C6 . . 123.2(2) ?
C3 C4 C5 . . 119.0(2) ?
C3 C4 H4A . . 120.5 ?
C5 C4 H4A . . 120.5 ?
C15 C14 C13 . . 123.5(2) ?
C15 C14 N3 . . 118.4(2) ?
C13 C14 N3 . . 118.1(2) ?
C14 C13 C12 . . 118.1(2) ?
C14 C13 H13A . . 120.9 ?
C12 C13 H13A . . 120.9 ?
C14 C15 C16 . . 118.3(2) ?
C14 C15 H15A . . 120.9 ?
C16 C15 H15A . . 120.9 ?
C8 C9 C10 . . 118.6(2) ?
C8 C9 H9A . . 120.7 ?
C10 C9 H9A . . 120.7 ?
C8 C7 C6 . . 118.7(2) ?
C8 C7 H7A . . 120.7 ?
C6 C7 H7A . . 120.7 ?
N2 C10 C9 . . 122.5(2) ?
N2 C10 H10A . . 118.8 ?
C9 C10 H10A . . 118.8 ?
N1 C1 C2 . . 123.0(2) ?
N1 C1 H1A . . 118.5 ?
C2 C1 H1A . . 118.5 ?
C9 C8 C7 . . 119.6(2) ?
C9 C8 H8A . . 120.2 ?
C7 C8 H8A . . 120.2 ?
C1 C2 C3 . . 118.4(2) ?
C1 C2 H2A . . 120.8 ?
C3 C2 H2A . . 120.8 ?
O5 N3 O6 . . 122.5(3) ?
O5 N3 C14 . . 117.9(3) ?
O6 N3 C14 . . 119.3(2) ?
C2 C3 C4 . . 119.5(2) ?
C2 C3 H3A . . 120.3 ?
C4 C3 H3A . . 120.3 ?
C17 O2 Co1 . . 138.15(16) ?
C19 O4 Co1 . 1_655 137.23(17) ?
Co2 O1W H1WA . . 109(2) ?
Co2 O1W H1WB . . 111(2) ?
H1WA O1W H1WB . . 109(2) ?
C32 O8 Co2 . . 92.74(15) ?
O8 C32 O9 . . 119.2(2) ?
O8 C32 C33 . . 120.5(2) ?
O9 C32 C33 . . 120.2(2) ?
C32 C33 H33A . . 109.5 ?
C32 C33 H33B . . 109.5 ?
H33A C33 H33B . . 109.5 ?
C32 C33 H33C . . 109.5 ?
H33A C33 H33C . . 109.5 ?
H33B C33 H33C . . 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
Co1 O2 . 2.0503(16) ?
Co1 O2 2_576 2.0503(16) ?
Co1 O9 2_576 2.1153(15) ?
Co1 O9 . 2.1153(15) ?
Co1 O4 1_455 2.1154(17) ?
Co1 O4 2_676 2.1154(17) ?
Co2 O1 . 2.0392(15) ?
Co2 O1W . 2.0831(18) ?
Co2 N1 . 2.1053(19) ?
Co2 N2 . 2.1249(19) ?
Co2 O8 . 2.1668(18) ?
Co2 O9 . 2.2382(16) ?
N1 C1 . 1.338(3) ?
N1 C5 . 1.350(3) ?
N2 C10 . 1.331(3) ?
N2 C6 . 1.345(3) ?
C6 C7 . 1.385(3) ?
C6 C5 . 1.487(3) ?
O1 C17 . 1.259(3) ?
O9 C32 . 1.281(3) ?
C11 C16 . 1.391(3) ?
C11 C12 . 1.395(3) ?
C11 H11A . 0.9300 ?
C17 O2 . 1.248(3) ?
C17 C16 . 1.508(3) ?
C16 C15 . 1.388(3) ?
C19 O3 . 1.244(3) ?
C19 O4 . 1.252(3) ?
C19 C12 . 1.510(3) ?
C12 C13 . 1.390(3) ?
C5 C4 . 1.384(3) ?
C4 C3 . 1.381(4) ?
C4 H4A . 0.9300 ?
C14 C15 . 1.375(3) ?
C14 C13 . 1.380(4) ?
C14 N3 . 1.471(3) ?
C13 H13A . 0.9300 ?
C15 H15A . 0.9300 ?
C9 C8 . 1.372(4) ?
C9 C10 . 1.380(4) ?
C9 H9A . 0.9300 ?
C7 C8 . 1.382(4) ?
C7 H7A . 0.9300 ?
C10 H10A . 0.9300 ?
C1 C2 . 1.377(4) ?
C1 H1A . 0.9300 ?
C8 H8A . 0.9300 ?
C2 C3 . 1.380(4) ?
C2 H2A . 0.9300 ?
N3 O5 . 1.199(3) ?
N3 O6 . 1.206(3) ?
C3 H3A . 0.9300 ?
O4 Co1 1_655 2.1154(17) ?
O1W H1WA . 0.826(10) ?
O1W H1WB . 0.824(10) ?
O8 C32 . 1.248(3) ?
C32 C33 . 1.493(4) ?
C33 H33A . 0.9600 ?
C33 H33B . 0.9600 ?
C33 H33C . 0.9600 ?
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
O1W H1WA O3 1_455 0.83(2) 1.99(2) 2.755(3) 154(2) yes
O1W H1WB O3 2_666 0.826(18) 1.96(2) 2.762(3) 163(3) yes
