#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/63/2016329.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_2016329
loop_
_publ_author_name
'Kukovec, Boris-Marko'
'Popović, Zora'
'Pavlović, Gordana'
_publ_section_title
;A new coordination mode of 6-methylnicotinic acid in
 trans-tetraaquabis(6-methylpyridine-3-carboxylato-κO)cobalt(II)
 tetrahydrate
;
_journal_coeditor_code           GD3165
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m615
_journal_page_last               m617
_journal_paper_doi               10.1107/S0108270107056570
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Co (C7 H6 N O2)2 (H2 O)4], 4H2 O'
_chemical_formula_moiety         'C14 H20 Co N2 O8, 4(H2 O)'
_chemical_formula_sum            'C14 H28 Co N2 O12'
_chemical_formula_weight         475.31
_chemical_name_common
;
 tetraaqua-trans-bis(6-methylnicotinato-O)cobalt(II)
tetrahydrate
;
_chemical_name_systematic
;
tetraaqua-trans-bis(6-methylpyridine-3-carboxylato-\kO)cobalt(II)
tetrahydrate
;
_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                86.829(2)
_cell_angle_beta                 78.746(3)
_cell_angle_gamma                65.357(3)
_cell_formula_units_Z            1
_cell_length_a                   7.0284(2)
_cell_length_b                   7.3655(2)
_cell_length_c                   11.4912(4)
_cell_measurement_reflns_used    12287
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      34.93
_cell_measurement_theta_min      3.99
_cell_volume                     530.07(3)
_computing_cell_refinement
'CrysAlis CCD or RED? (Oxford Diffraction, 2007)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and Mercury (Macrae et al.,  2006)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur2 diffractometer with Sapphire 3 CCD detector'
_diffrn_measurement_method       ω-scan
_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  0.0156
_diffrn_reflns_av_sigmaI/netI    0.0123
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14868
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         4.01
_diffrn_standards_interval_count '1 ref frame per 50 dc frames'
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2007)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             249
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.819
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3062
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0339
_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)+(0.0592P)²+0.0689P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0892
_reflns_number_gt                2783
_reflns_number_total             3062
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            gd3165.cif
_cod_data_source_block           I
_cod_database_code               2016329
_cod_database_fobs_code          2016329
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 0.0000 0.5000 0.5000 0.02579(9) Uani d S 1
N N1 -0.19146(18) 0.77732(17) -0.04924(9) 0.0299(2) Uani d . 1
O O1 -0.10712(16) 0.56022(16) 0.34141(8) 0.0342(2) Uani d . 1
O O2 0.10956(16) 0.68928(16) 0.23789(9) 0.0342(2) Uani d . 1
O O3 0.27610(15) 0.54722(16) 0.42744(9) 0.0336(2) Uani d D 1
H H31 0.303(4) 0.628(4) 0.470(2) 0.065(7) Uiso d D 1
H H32 0.241(4) 0.610(4) 0.356(2) 0.071(7) Uiso d D 1
O O4 0.1713(2) 0.19649(16) 0.44155(10) 0.0421(2) Uani d D 1
H H41 0.136(3) 0.153(3) 0.390(2) 0.049(6) Uiso d D 1
H H42 0.223(3) 0.103(3) 0.4783(19) 0.048(6) Uiso d D 1
O O5 0.3325(2) 0.8246(2) 0.56128(11) 0.0454(3) Uani d D 1
H H51 0.447(4) 0.759(4) 0.576(2) 0.075(8) Uiso d D 1
H H52 0.244(5) 0.831(5) 0.622(3) 0.089(9) Uiso d D 1
O O6 0.0242(2) 0.08979(18) 0.26089(10) 0.0432(3) Uani d D 1
H H61 0.082(3) 0.136(3) 0.1935(19) 0.050(5) Uiso d D 1
H H62 0.058(4) -0.030(4) 0.253(2) 0.069(7) Uiso d D 1
C C1 -0.09323(19) 0.74354(19) 0.04328(11) 0.0279(2) Uani d . 1
H H1 0.0301 0.7649 0.0346 0.034 Uiso calc R 1
C C2 -0.16503(18) 0.67819(17) 0.15192(10) 0.0248(2) Uani d . 1
C C3 -0.3510(2) 0.6491(2) 0.16393(11) 0.0318(2) Uani d . 1
H H3 -0.4043 0.6047 0.2349 0.038 Uiso calc R 1
C C4 -0.4557(2) 0.6867(2) 0.06949(12) 0.0336(3) Uani d . 1
H H4 -0.5817 0.6704 0.0768 0.040 Uiso calc R 1
C C5 -0.3711(2) 0.74921(18) -0.03710(11) 0.0284(2) Uani d . 1
C C6 -0.04491(18) 0.64040(17) 0.25142(10) 0.0249(2) Uani d . 1
C C7 -0.4755(2) 0.7869(2) -0.14280(13) 0.0378(3) Uani d . 1
H H71 -0.3905 0.6836 -0.2022 0.057 Uiso calc R 1
H H72 -0.4888 0.9141 -0.1744 0.057 Uiso calc R 1
H H73 -0.6145 0.7872 -0.1196 0.057 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'
Co Co 0.3494 0.9721 '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'
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 O1 . 2_566 180.0 no
O1 Co1 O3 . . 92.11(4) yes
O1 Co1 O3 2_566 . 87.89(4) no
O1 Co1 O3 . 2_566 87.89(4) yes
O1 Co1 O3 2_566 2_566 92.11(4) no
O3 Co1 O3 . 2_566 180.0 no
O1 Co1 O4 . . 88.30(4) yes
O1 Co1 O4 2_566 . 91.70(4) no
O3 Co1 O4 . . 88.41(5) yes
O3 Co1 O4 2_566 . 91.59(5) yes
O1 Co1 O4 . 2_566 91.70(4) yes
O1 Co1 O4 2_566 2_566 88.30(4) no
O3 Co1 O4 . 2_566 91.59(5) no
O3 Co1 O4 2_566 2_566 88.41(5) no
O4 Co1 O4 . 2_566 180.0 no
C1 N1 C5 . . 118.58(11) no
C6 O1 Co1 . . 128.79(8) no
Co1 O3 H31 . . 115.6(16) no
Co1 O3 H32 . . 101.6(17) no
H31 O3 H32 . . 108(2) no
Co1 O4 H41 . . 120.2(15) no
Co1 O4 H42 . . 128.7(16) no
H41 O4 H42 . . 103(2) no
H51 O5 H52 . . 107(3) no
H61 O6 H62 . . 110(2) no
N1 C1 C2 . . 123.70(11) no
N1 C1 H1 . . 118.2 no
C2 C1 H1 . . 118.2 no
C3 C2 C1 . . 117.46(11) no
C3 C2 C6 . . 121.70(10) no
C1 C2 C6 . . 120.83(11) no
C4 C3 C2 . . 119.30(11) no
C4 C3 H3 . . 120.4 no
C2 C3 H3 . . 120.4 no
C3 C4 C5 . . 119.58(12) no
C3 C4 H4 . . 120.2 no
C5 C4 H4 . . 120.2 no
N1 C5 C4 . . 121.36(11) no
N1 C5 C7 . . 117.06(12) no
C4 C5 C7 . . 121.58(12) no
O1 C6 O2 . . 125.66(11) no
O1 C6 C2 . . 116.49(10) no
O2 C6 C2 . . 117.85(10) no
C5 C7 H71 . . 109.5 no
C5 C7 H72 . . 109.5 no
H71 C7 H72 . . 109.5 no
C5 C7 H73 . . 109.5 no
H71 C7 H73 . . 109.5 no
H72 C7 H73 . . 109.5 no
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 . 2.0621(9) yes
Co1 O1 2_566 2.0621(9) no
Co1 O3 . 2.1169(9) yes
Co1 O3 2_566 2.1169(9) no
Co1 O4 . 2.1223(11) yes
Co1 O4 2_566 2.1223(11) no
N1 C1 . 1.3352(16) no
N1 C5 . 1.3424(17) no
O1 C6 . 1.2572(14) yes
O2 C6 . 1.2595(15) yes
O3 H31 . 0.89(2) no
O3 H32 . 0.94(2) no
O4 H41 . 0.82(2) no
O4 H42 . 0.78(2) no
O5 H51 . 0.79(3) no
O5 H52 . 0.83(3) no
O6 H61 . 0.92(2) no
O6 H62 . 0.82(3) no
C1 C2 . 1.3910(16) no
C1 H1 . 0.9300 no
C2 C3 . 1.3907(17) no
C2 C6 . 1.4977(16) no
C3 C4 . 1.3797(18) no
C3 H3 . 0.9300 no
C4 C5 . 1.3955(18) no
C4 H4 . 0.9300 no
C5 C7 . 1.4941(18) no
C7 H71 . 0.9600 no
C7 H72 . 0.9600 no
C7 H73 . 0.9600 no
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
O3 H31 O5 1_555 0.90(3) 1.93(3) 2.821(2) 174(3) yes
O3 H32 O2 . 0.94(2) 1.73(3) 2.633(2) 159(3) yes
O4 H41 O6 1_555 0.81(2) 1.97(2) 2.774(2) 171(2) yes
O4 H42 O5 1_545 0.78(2) 2.11(2) 2.878(2) 169(2) yes
O5 H51 O3 2_666 0.79(3) 2.28(3) 2.984(2) 148(3) yes
O5 H52 O6 2_566 0.83(4) 1.97(4) 2.772(2) 163(3) yes
O6 H61 N1 2_565 0.92(2) 1.88(2) 2.799(2) 176(2) yes
O6 H62 O2 1_545 0.82(3) 1.96(3) 2.771(2) 175(3) yes
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
_geom_torsion_publ_flag
O3 Co1 O1 C6 . -14.28(11) no
O3 Co1 O1 C6 2_566 165.72(11) no
O4 Co1 O1 C6 . -102.63(12) no
O4 Co1 O1 C6 2_566 77.37(12) no
C5 N1 C1 C2 . 0.79(19) no
N1 C1 C2 C3 . -0.70(19) no
N1 C1 C2 C6 . 179.09(11) no
C1 C2 C3 C4 . -0.37(19) no
C6 C2 C3 C4 . 179.84(11) no
C2 C3 C4 C5 . 1.3(2) no
C1 N1 C5 C4 . 0.20(19) no
C1 N1 C5 C7 . -179.52(11) no
C3 C4 C5 N1 . -1.2(2) no
C3 C4 C5 C7 . 178.47(12) no
Co1 O1 C6 O2 . 5.01(19) no
Co1 O1 C6 C2 . -175.66(8) no
C3 C2 C6 O1 . 7.65(17) no
C1 C2 C6 O1 . -172.13(11) no
C3 C2 C6 O2 . -172.97(12) no
C1 C2 C6 O2 . 7.24(17) no
