##############################################################################
### ###
### Electronic paper (Acta Crystallographica Section E) ###
### ###
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# #
# This CIF contains the data in a paper accepted for publication in Acta #
# Crystallographica Section E. It conforms to the requirements of Notes #
# for Authors for Section E, and has been peer reviewed under the auspices #
# of the IUCr Commission on Journals. #
# #
# Full details of the Crystallographic Information File format #
# are given in the paper "The Crystallographic Information File (CIF): #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H. #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. #
# #
# The current version of the core CIF dictionary is obtainable from #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.4. #
# #
# Software is freely available for graphical display of the structure(s) in #
# this CIF. For information consult the CIF home page http://www.iucr.org/ #
# cif/home.html #
# #
# This file may be used for bona fide research purposes within the #
# scientific community so long as proper attribution is given to the journal #
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data_I
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
Diaquabis(pyridine-2-carboxylato-\k^2^N,O)cobalt(II)
;
_chemical_name_common ?
_chemical_formula_moiety "C12 H12 Co N2 O6"
_chemical_formula_sum 'C12 H12 Co N2 O6'
_chemical_formula_iupac '[Co (C6 H4 N O2)2 (H2 O)2]'
_chemical_formula_weight 339.17
_chemical_melting_point ?
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/n'
_symmetry_space_group_name_Hall '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 11.7401(3)
_cell_length_b 8.9994(6)
_cell_length_c 14.9211(3)
_cell_angle_alpha 90.00
_cell_angle_beta 105.985(2)
_cell_angle_gamma 90.00
_cell_volume 1515.52(11)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 2863
_cell_measurement_theta_min 2.595
_cell_measurement_theta_max 23.777
_cell_measurement_temperature 273(2)
_exptl_crystal_description plate
_exptl_crystal_colour pink
_exptl_crystal_size_max 0.24
_exptl_crystal_size_mid 0.18
_exptl_crystal_size_min 0.08
_exptl_crystal_density_diffrn 1.486
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 692
_exptl_absorpt_coefficient_mu 1.159
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_absorpt_correction_T_min 0.7700
_exptl_absorpt_correction_T_max 0.9181
_exptl_special_details
;
;
_diffrn_ambient_temperature 273(2)
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker APEXII area-detector'
_diffrn_measurement_method '\f and \w'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 9384
_diffrn_reflns_av_R_equivalents 0.0418
_diffrn_reflns_av_sigmaI/netI 0.0618
_diffrn_reflns_theta_min 1.96
_diffrn_reflns_theta_max 26.00
_diffrn_reflns_theta_full 26.00
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 17
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_reflns_number_total 2926
_reflns_number_gt 2065
_reflns_threshold_expression I>2\s(I)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.0824
_refine_ls_R_factor_gt 0.0597
_refine_ls_wR_factor_gt 0.2010
_refine_ls_wR_factor_ref 0.2269
_refine_ls_goodness_of_fit_ref 1.072
_refine_ls_restrained_S_all 1.075
_refine_ls_number_reflns 2926
_refine_ls_number_parameters 200
_refine_ls_number_restraints 6
_refine_ls_hydrogen_treatment mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.152P)^2^+0.1958P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.829
_refine_diff_density_min -0.623
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
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'
_computing_data_collection 'SMART (Siemens, 1996)'
_computing_cell_refinement 'SAINT (Siemens, 1996)'
_computing_data_reduction 'SAINT (Siemens, 1996)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)'
_computing_publication_material 'SHELXTL (Sheldrick, 2008)'
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 0.74558(5) 0.85905(7) 0.62775(4) 0.0500(3) Uani d . 1 . .
O O1 0.8193(3) 0.7460(4) 0.7578(2) 0.0528(8) Uani d D 1 . .
H H1A 0.7662 0.7036 0.7737 0.079 Uiso calc RD 1 . .
H H1B 0.8854(17) 0.719(5) 0.773(3) 0.065(16) Uiso d D 1 . .
O O2 0.5921(3) 0.8896(4) 0.6792(3) 0.0562(9) Uani d D 1 . .
H H2A 0.5826 0.8156 0.7083 0.084 Uiso calc RD 1 . .
H H2B 0.546(3) 0.953(3) 0.673(3) 0.035(12) Uiso d D 1 . .
O O3 0.6510(3) 0.9270(3) 0.48901(19) 0.0497(8) Uani d . 1 . .
O O4 0.5390(3) 0.8577(3) 0.3503(2) 0.0560(9) Uani d . 1 . .
O O5 0.8183(3) 1.0767(4) 0.6673(2) 0.0512(8) Uani d . 1 . .
O O6 0.9716(3) 1.2287(4) 0.6898(3) 0.0724(11) Uani d . 1 . .
N N1 0.9333(3) 0.8598(4) 0.6113(3) 0.0504(9) Uani d . 1 . .
N N2 0.6905(3) 0.6452(4) 0.5461(2) 0.0406(8) Uani d . 1 . .
C C1 0.6032(3) 0.8310(5) 0.4295(3) 0.0423(9) Uani d . 1 . .
C C2 0.6267(3) 0.6693(5) 0.4583(3) 0.0392(9) Uani d . 1 . .
C C3 0.5838(4) 0.5535(5) 0.3968(3) 0.0533(11) Uani d . 1 . .
H H3 0.5424 0.5722 0.3351 0.064 Uiso calc R 1 . .
C C4 0.6040(4) 0.4115(6) 0.4293(3) 0.0552(11) Uani d . 1 . .
H H4 0.5727 0.3319 0.3906 0.066 Uiso calc R 1 . .
C C5 0.6700(4) 0.3862(5) 0.5184(4) 0.0552(12) Uani d . 1 . .
H H5 0.6864 0.2897 0.5404 0.066 Uiso calc R 1 . .
C C6 0.7120(4) 0.5054(5) 0.5755(3) 0.0495(10) Uani d . 1 . .
H H6 0.7569 0.4880 0.6364 0.059 Uiso calc R 1 . .
C C7 0.9224(4) 1.1095(5) 0.6665(3) 0.0513(11) Uani d . 1 . .
C C8 0.9904(4) 0.9869(5) 0.6340(3) 0.0489(11) Uani d . 1 . .
C C9 1.1060(4) 1.0058(7) 0.6312(4) 0.0704(15) Uani d . 1 . .
H H9 1.1443 1.0961 0.6485 0.085 Uiso calc R 1 . .
C C10 1.1635(6) 0.8917(7) 0.6029(6) 0.091(2) Uani d . 1 . .
H H10 1.2403 0.9039 0.5983 0.109 Uiso calc R 1 . .
C C11 1.1064(6) 0.7581(8) 0.5811(6) 0.102(2) Uani d . 1 . .
H H11 1.1445 0.6768 0.5639 0.123 Uiso calc R 1 . .
C C12 0.9906(5) 0.7476(6) 0.5856(5) 0.0772(17) Uani d . 1 . .
H H12 0.9510 0.6578 0.5698 0.093 Uiso calc R 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Co1 0.0509(5) 0.0450(5) 0.0472(5) -0.0007(3) 0.0018(3) -0.0005(2)
O1 0.0397(16) 0.060(2) 0.0502(18) 0.0013(15) -0.0015(13) 0.0150(14)
O2 0.056(2) 0.0450(19) 0.070(2) 0.0125(16) 0.0209(17) 0.0143(16)
O3 0.0515(17) 0.0412(18) 0.0466(17) -0.0020(13) -0.0031(13) 0.0045(13)
O4 0.0550(19) 0.052(2) 0.0467(18) 0.0079(14) -0.0106(14) 0.0083(13)
O5 0.0467(17) 0.0448(18) 0.0613(19) -0.0019(14) 0.0135(14) -0.0096(15)
O6 0.078(2) 0.059(2) 0.089(3) -0.0299(19) 0.037(2) -0.031(2)
N1 0.049(2) 0.046(2) 0.059(2) -0.0010(17) 0.0189(18) -0.0046(17)
N2 0.0418(18) 0.037(2) 0.0366(18) -0.0012(14) 0.0011(14) 0.0024(13)
C1 0.0331(19) 0.049(2) 0.040(2) 0.0023(17) 0.0035(16) 0.0025(18)
C2 0.0334(19) 0.041(2) 0.039(2) -0.0012(16) 0.0032(15) -0.0034(17)
C3 0.051(2) 0.053(3) 0.046(2) 0.005(2) -0.0033(18) -0.008(2)
C4 0.056(3) 0.044(3) 0.061(3) 0.002(2) 0.008(2) -0.012(2)
C5 0.064(3) 0.041(3) 0.064(3) 0.001(2) 0.023(2) -0.001(2)
C6 0.057(2) 0.044(3) 0.044(2) 0.001(2) 0.0068(19) 0.0031(19)
C7 0.059(3) 0.055(3) 0.039(2) -0.011(2) 0.0124(19) -0.0056(19)
C8 0.050(2) 0.055(3) 0.042(2) 0.006(2) 0.0146(18) 0.0039(19)
C9 0.058(3) 0.073(4) 0.086(4) -0.008(3) 0.027(3) -0.001(3)
C10 0.069(4) 0.085(5) 0.134(6) -0.001(4) 0.054(4) 0.006(4)
C11 0.085(4) 0.079(5) 0.165(8) 0.016(4) 0.074(5) -0.007(5)
C12 0.076(4) 0.052(3) 0.114(5) -0.001(3) 0.043(3) -0.012(3)
_geom_special_details
;
All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix. The cell e.s.d.'s
are taken into account individually in the estimation of e.s.d.'s in
distances, angles and torsion angles; correlations between e.s.d.'s in cell
parameters are only used when they are defined by crystal symmetry. An
approximate (isotropic) treatment of cell e.s.d.'s is used for estimating
e.s.d.'s involving l.s. planes.
;
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 O1 . 2.150(3) yes
Co1 O2 . 2.162(3) yes
Co1 O3 . 2.151(3) yes
Co1 O5 . 2.153(3) yes
Co1 N1 . 2.284(4) yes
Co1 N2 . 2.274(3) yes
O1 H1A . 0.8200 ?
O1 H1B . 0.784(18) ?
O2 H2A . 0.8200 ?
O2 H2B . 0.771(16) ?
O3 C1 . 1.255(5) ?
O4 C1 . 1.238(5) ?
O5 C7 . 1.261(5) ?
O6 C7 . 1.222(5) ?
N1 C8 . 1.321(6) ?
N1 C12 . 1.327(6) ?
N2 C6 . 1.334(5) ?
N2 C2 . 1.335(5) ?
C1 C2 . 1.521(6) ?
C2 C3 . 1.389(6) ?
C3 C4 . 1.365(7) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.361(7) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.374(6) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
C7 C8 . 1.517(6) ?
C8 C9 . 1.380(7) ?
C9 C10 . 1.359(8) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.371(9) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.383(8) ?
C11 H11 . 0.9300 ?
C12 H12 . 0.9300 ?
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
O1 Co1 O2 . . 84.68(13) yes
O1 Co1 O3 . . 167.36(12) yes
O1 Co1 O5 . . 98.78(12) yes
O2 Co1 O3 . . 92.63(13) yes
O2 Co1 O5 . . 95.35(13) yes
O3 Co1 O5 . . 93.75(12) yes
O1 Co1 N1 . . 86.44(14) yes
O2 Co1 N1 . . 163.96(15) yes
O3 Co1 N1 . . 98.83(14) yes
O5 Co1 N1 . . 72.84(12) yes
O1 Co1 N2 . . 93.86(12) yes
O2 Co1 N2 . . 98.99(14) yes
O3 Co1 N2 . . 74.33(12) yes
O5 Co1 N2 . . 161.68(13) yes
N1 Co1 N2 . . 94.91(13) yes
Co1 O1 H1A . . 109.5 ?
Co1 O1 H1B . . 122(3) ?
H1A O1 H1B . . 123.0 ?
Co1 O2 H2A . . 109.5 ?
Co1 O2 H2B . . 132(2) ?
H2A O2 H2B . . 118.0 ?
C1 O3 Co1 . . 119.8(3) ?
C7 O5 Co1 . . 121.5(3) ?
C8 N1 C12 . . 118.1(4) ?
C8 N1 Co1 . . 114.3(3) ?
C12 N1 Co1 . . 127.5(3) ?
C6 N2 C2 . . 118.6(4) ?
C6 N2 Co1 . . 128.5(3) ?
C2 N2 Co1 . . 112.8(3) ?
O4 C1 O3 . . 125.3(4) ?
O4 C1 C2 . . 118.2(4) ?
O3 C1 C2 . . 116.6(4) ?
N2 C2 C3 . . 122.0(4) ?
N2 C2 C1 . . 116.2(3) ?
C3 C2 C1 . . 121.8(4) ?
C4 C3 C2 . . 118.2(4) ?
C4 C3 H3 . . 120.9 ?
C2 C3 H3 . . 120.9 ?
C5 C4 C3 . . 120.0(4) ?
C5 C4 H4 . . 120.0 ?
C3 C4 H4 . . 120.0 ?
C4 C5 C6 . . 119.1(5) ?
C4 C5 H5 . . 120.5 ?
C6 C5 H5 . . 120.5 ?
N2 C6 C5 . . 122.0(4) ?
N2 C6 H6 . . 119.0 ?
C5 C6 H6 . . 119.0 ?
O6 C7 O5 . . 125.9(5) ?
O6 C7 C8 . . 118.7(4) ?
O5 C7 C8 . . 115.4(4) ?
N1 C8 C9 . . 122.2(4) ?
N1 C8 C7 . . 116.0(4) ?
C9 C8 C7 . . 121.9(5) ?
C10 C9 C8 . . 119.5(5) ?
C10 C9 H9 . . 120.2 ?
C8 C9 H9 . . 120.2 ?
C9 C10 C11 . . 119.0(5) ?
C9 C10 H10 . . 120.5 ?
C11 C10 H10 . . 120.5 ?
C10 C11 C12 . . 118.1(6) ?
C10 C11 H11 . . 120.9 ?
C12 C11 H11 . . 120.9 ?
N1 C12 C11 . . 123.0(6) ?
N1 C12 H12 . . 118.5 ?
C11 C12 H12 . . 118.5 ?
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 H1B O4 4_676 0.784(18) 1.98(3) 2.733(4) 161(4) yes
O1 H1A O5 2_646 0.82 1.88 2.679(4) 164 yes
O2 H2B O4 3_676 0.771(16) 1.959(16) 2.712(4) 166(3) yes
O2 H2A O6 2_646 0.82 1.96 2.699(5) 149 yes
data_global
_journal_date_recd_electronic 2008-04-07
_journal_date_accepted 2008-04-16
_journal_name_full 'Acta Crystallographica, Section E'
_journal_year 2008
_journal_volume 64
_journal_issue 5
_journal_page_first m685
_journal_page_last m686
_journal_paper_category QM
_journal_coeditor_code HK2450
_publ_contact_author_name 'G. S. Huang'
_publ_contact_author_address
;
College of Chemistry & Chemical Engineering,
Jinggangshan University,
Jian 343009, People^,^s Republic of China
;
_publ_contact_author_email gshuang08@126.com
_publ_contact_author_fax +86-796-8100490
_publ_contact_author_phone +86-796-8100490
_publ_section_title
;
Diaquabis(pyridine-2-carboxylato-\k^2^N,O)cobalt(II)
;
loop_
_publ_author_name
_publ_author_address
'G. S. Huang'
;
College of Chemistry & Chemical Engineering
Provincial key laboratory of Coordination Chemistry
Jinggangshan University,
Jian 343009
People's Republic of China
;