#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/52/2205266.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_2205266
loop_
_publ_author_name
'Fu, Ai-Yun'
'Wang, Da-Qi'
_publ_section_title
;
 Tris(pyridine-2-carboxylato-κ²O,N)cobalt(III)
 monohydrate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m481
_journal_page_last               m482
_journal_paper_doi               10.1107/S160053680500317X
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Co (C6 H4 N1 O2)3], H2 O'
_chemical_formula_moiety         'C18 H12 Co N3 O6, H2 O'
_chemical_formula_sum            'C18 H14 Co N3 O7'
_chemical_formula_weight         443.25
_chemical_name_systematic
;
Tris(pyridine-2-carboxylato-κ²0,N)cobalt(III) monohydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.829(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.654(18)
_cell_length_b                   8.530(5)
_cell_length_c                   13.801(8)
_cell_measurement_reflns_used    1193
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20.267
_cell_measurement_theta_min      2.486
_cell_volume                     3473(4)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and 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  0.0587
_diffrn_reflns_av_sigmaI/netI    0.1032
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9671
_diffrn_reflns_theta_full        26.47
_diffrn_reflns_theta_max         26.47
_diffrn_reflns_theta_min         1.38
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.039
_exptl_absorpt_correction_T_max  0.835
_exptl_absorpt_correction_T_min  0.760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1997)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.485
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         3589
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0501
_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)] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0656
_reflns_number_gt                2020
_reflns_number_total             3589
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb6144.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'C 2/c'
_cod_database_code               2205266
_cod_database_fobs_code          2205266
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_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_type_symbol
Co1 0.387460(17) 0.21873(5) 0.87334(3) 0.03472(15) Uani d . 1 Co
N1 0.38357(9) 0.2424(3) 1.01036(17) 0.0309(7) Uani d . 1 N
N2 0.33464(9) 0.0897(3) 0.8503(2) 0.0329(7) Uani d . 1 N
N3 0.44347(10) 0.3284(3) 0.88006(17) 0.0339(7) Uani d . 1 N
O1 0.34972(8) 0.3952(3) 0.86091(15) 0.0385(6) Uani d . 1 O
O2 0.30261(9) 0.5311(3) 0.94475(18) 0.0604(8) Uani d . 1 O
O3 0.38711(8) 0.2182(3) 0.73697(15) 0.0405(6) Uani d . 1 O
O4 0.34080(9) 0.1683(3) 0.60350(17) 0.0628(9) Uani d . 1 O
O5 0.42424(8) 0.0394(3) 0.88591(15) 0.0402(6) Uani d . 1 O
O6 0.49517(9) -0.0402(3) 0.87981(19) 0.0582(8) Uani d . 1 O
O7 0.39030(12) 0.2557(3) 0.4458(2) 0.0775(9) Uani d D 1 O
C1 0.33287(13) 0.4382(4) 0.9402(3) 0.0420(10) Uani d . 1 C
C2 0.35444(12) 0.3561(4) 1.0286(3) 0.0342(9) Uani d . 1 C
C3 0.34641(15) 0.3915(5) 1.1230(3) 0.0491(12) Uani d . 1 C
C4 0.36846(16) 0.3099(5) 1.1984(3) 0.0537(12) Uani d . 1 C
C5 0.39892(15) 0.1985(5) 1.1794(3) 0.0476(11) Uani d . 1 C
C6 0.40585(13) 0.1656(5) 1.0840(3) 0.0402(10) Uani d . 1 C
C7 0.35117(14) 0.1619(4) 0.6921(3) 0.0398(10) Uani d . 1 C
C8 0.32015(12) 0.0820(4) 0.7549(3) 0.0338(9) Uani d . 1 C
C9 0.28190(15) 0.0059(5) 0.7221(3) 0.0514(12) Uani d . 1 C
C10 0.25745(16) -0.0690(5) 0.7857(4) 0.0600(14) Uani d . 1 C
C11 0.27208(15) -0.0663(5) 0.8828(4) 0.0550(12) Uani d . 1 C
C12 0.31034(14) 0.0165(5) 0.9128(3) 0.0436(11) Uani d . 1 C
C13 0.46680(14) 0.0627(5) 0.8806(2) 0.0386(10) Uani d . 1 C
C14 0.47919(12) 0.2304(4) 0.8786(2) 0.0348(9) Uani d . 1 C
C15 0.52188(14) 0.2874(5) 0.8750(3) 0.0444(10) Uani d . 1 C
C16 0.52897(16) 0.4446(6) 0.8730(3) 0.0495(12) Uani d . 1 C
C17 0.49301(17) 0.5447(6) 0.8751(3) 0.0471(11) Uani d . 1 C
C18 0.45050(15) 0.4823(5) 0.8784(3) 0.0441(11) Uani d . 1 C
H1 0.3284(10) 0.467(3) 1.132(2) 0.033(11) Uiso d . 1 H
H2 0.3611(10) 0.330(3) 1.262(2) 0.036(10) Uiso d . 1 H
H3 0.4144(10) 0.133(3) 1.231(2) 0.034(10) Uiso d . 1 H
H4 0.4270(10) 0.087(3) 1.0652(19) 0.033(10) Uiso d . 1 H
H5 0.2744(10) -0.002(3) 0.662(2) 0.022(10) Uiso d . 1 H
H6 0.2311(11) -0.119(4) 0.762(2) 0.041(11) Uiso d . 1 H
H7 0.2579(12) -0.123(4) 0.937(2) 0.063(12) Uiso d . 1 H
H8 0.3233(10) 0.022(3) 0.980(2) 0.035(10) Uiso d . 1 H
H9 0.5435(10) 0.216(3) 0.8729(19) 0.029(10) Uiso d . 1 H
H10 0.5576(11) 0.480(4) 0.867(2) 0.043(11) Uiso d . 1 H
H11 0.4935(11) 0.651(3) 0.873(2) 0.044(12) Uiso d . 1 H
H12 0.4244(11) 0.536(4) 0.881(2) 0.050 Uiso d . 1 H
H13 0.3733(9) 0.239(3) 0.4941(17) 0.050 Uiso d D 1 H
H14 0.4062(10) 0.170(2) 0.437(2) 0.050 Uiso d D 1 H
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
_geom_angle_publ_flag
O1 Co1 O5 178.85(11) y
O1 Co1 O3 88.14(10) y
O5 Co1 O3 91.99(10) y
O1 Co1 N3 96.90(13) y
O5 Co1 N3 84.25(13) y
O3 Co1 N3 88.04(10) y
O1 Co1 N2 88.59(12) y
O5 Co1 N2 90.28(12) y
O3 Co1 N2 84.91(11) y
N3 Co1 N2 170.93(11) y
O1 Co1 N1 84.86(11) y
O5 Co1 N1 95.01(11) y
O3 Co1 N1 172.98(12) y
N3 Co1 N1 92.28(11) y
N2 Co1 N1 95.41(11) y
C6 N1 C2 119.6(3) ?
C6 N1 Co1 128.9(3) ?
C2 N1 Co1 111.5(2) ?
C12 N2 C8 118.1(3) ?
C12 N2 Co1 130.4(3) ?
C8 N2 Co1 111.4(2) ?
C18 N3 C14 119.1(3) ?
C18 N3 Co1 128.5(3) ?
C14 N3 Co1 112.2(2) ?
C1 O1 Co1 115.3(2) ?
C7 O3 Co1 114.1(2) ?
C13 O5 Co1 115.6(2) ?
H13 O7 H14 109(2) ?
O2 C1 O1 125.6(4) ?
O2 C1 C2 121.7(4) ?
O1 C1 C2 112.7(3) ?
N1 C2 C3 120.8(4) ?
N1 C2 C1 114.6(3) ?
C3 C2 C1 124.6(4) ?
C4 C3 C2 119.5(4) ?
C4 C3 H1 123(2) ?
C2 C3 H1 118(2) ?
C5 C4 C3 119.2(4) ?
C5 C4 H2 122.1(19) ?
C3 C4 H2 118.7(19) ?
C4 C5 C6 119.6(4) ?
C4 C5 H3 122.2(17) ?
C6 C5 H3 118.0(17) ?
N1 C6 C5 121.2(4) ?
N1 C6 H4 114.9(16) ?
C5 C6 H4 123.9(17) ?
O4 C7 O3 125.4(4) ?
O4 C7 C8 119.4(4) ?
O3 C7 C8 115.2(3) ?
N2 C8 C9 121.9(4) ?
N2 C8 C7 113.1(3) ?
C9 C8 C7 125.0(4) ?
C8 C9 C10 119.9(4) ?
C8 C9 H5 120(2) ?
C10 C9 H5 120(2) ?
C9 C10 C11 119.4(4) ?
C9 C10 H6 118(2) ?
C11 C10 H6 122(2) ?
C12 C11 C10 118.5(4) ?
C12 C11 H7 114(2) ?
C10 C11 H7 127(2) ?
N2 C12 C11 122.2(4) ?
N2 C12 H8 114.0(17) ?
C11 C12 H8 123.7(17) ?
O6 C13 O5 124.8(4) ?
O6 C13 C14 121.7(4) ?
O5 C13 C14 113.4(3) ?
N3 C14 C15 120.9(4) ?
N3 C14 C13 113.7(3) ?
C15 C14 C13 125.5(4) ?
C16 C15 C14 120.0(4) ?
C16 C15 H9 124(2) ?
C14 C15 H9 116(2) ?
C15 C16 C17 119.5(4) ?
C15 C16 H10 118(2) ?
C17 C16 H10 122(2) ?
C16 C17 C18 118.6(4) ?
C16 C17 H11 128(2) ?
C18 C17 H11 114(2) ?
N3 C18 C17 122.0(4) ?
N3 C18 H12 111(2) ?
C17 C18 H12 127(2) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 O1 1.873(2) y
Co1 O5 1.877(2) y
Co1 O3 1.881(2) y
Co1 N3 1.900(3) y
Co1 N2 1.914(3) y
Co1 N1 1.917(3) y
N1 C6 1.328(4) ?
N1 C2 1.339(4) ?
N2 C12 1.334(4) ?
N2 C8 1.345(4) ?
N3 C18 1.330(4) ?
N3 C14 1.351(4) ?
O1 C1 1.301(4) ?
O2 C1 1.204(4) ?
O3 C7 1.271(4) ?
O4 C7 1.231(4) ?
O5 C13 1.287(4) ?
O6 C13 1.217(4) ?
O7 H13 0.887(10) ?
O7 H14 0.886(10) ?
C1 C2 1.494(5) ?
C2 C3 1.381(5) ?
C3 C4 1.362(5) ?
C3 H1 0.85(3) ?
C4 C5 1.355(5) ?
C4 H2 0.95(3) ?
C5 C6 1.381(5) ?
C5 H3 0.98(3) ?
C6 H4 0.97(3) ?
C7 C8 1.491(5) ?
C8 C9 1.345(5) ?
C9 C10 1.354(5) ?
C9 H5 0.84(3) ?
C10 C11 1.367(5) ?
C10 H6 0.92(3) ?
C11 C12 1.365(5) ?
C11 H7 1.02(3) ?
C12 H8 0.97(3) ?
C13 C14 1.478(5) ?
C14 C15 1.362(5) ?
C15 C16 1.358(5) ?
C15 H9 0.89(3) ?
C16 C17 1.369(5) ?
C16 H10 0.91(3) ?
C17 C18 1.373(5) ?
C17 H11 0.91(3) ?
C18 H12 0.90(3) ?
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
O7 H14 O5 6 0.886(10) 2.012(15) 2.864(4) 161(3)
O7 H13 O4 . 0.887(10) 1.966(12) 2.845(4) 171(3)
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
C8 N2 N3 C14 -91.7(3)
O5 Co1 N1 C2 -173.3(2)
O1 Co1 O3 C7 -77.9(3)
