#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/94/2019468.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_2019468
loop_
_publ_author_name
'Harvey, Miguel Angel'
'Suarez, Sebastián'
'Doctorovich, Fabio'
'Cukiernik, Fabio D.'
'Baggio, Ricardo'
_publ_section_title
;
 The structure of {[Co(pht)(bpy)(H₂O)]·3H₂O}ₙ (pht is
 phthalate and bpy is 4,4'-bipyridine) and the role of solvent water
 clusters in structure stability
;
_journal_coeditor_code           YF3058
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              440
_journal_page_last               444
_journal_paper_doi               10.1107/S2053229614006950
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Co (C8 H4 O4) (C10 H8 N2) (H2 O)] , 3H2 O'
_chemical_formula_moiety         'C18 H14 Co  N2 O5, 3(H2 O)'
_chemical_formula_sum            'C18 H20 Co N2 O8'
_chemical_formula_weight         451.30
_chemical_name_systematic
'Poly[[aqua(μ-benzene-1,2-dicarboxylato-κ³O¹,O²:O¹)(μ-4,4'-bipyridine-κ²N:N')cobalt(II)] trihydrate]'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.564(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.0975(6)
_cell_length_b                   8.4039(3)
_cell_length_c                   11.3732(6)
_cell_measurement_reflns_used    3445
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      3.76
_cell_volume                     956.85(10)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'Oxford Gemini S Ultra CCD area-detector'
_diffrn_measurement_method       'ω scans, thick slices'
_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  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14398
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.86
_diffrn_reflns_theta_min         3.60
_exptl_absorpt_coefficient_mu    0.947
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlisPro; Oxford Diffraction, 2009)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             466
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.310
_refine_ls_abs_structure_details 'Flack (1983), with 2206 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.016(12)
_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     286
_refine_ls_number_reflns         4451
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0448P)²+0.4467P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                4096
_reflns_number_total             4451
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            yf3058sup1.cf
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2019468.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2019468
_cod_database_fobs_code          2019468
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -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_symmetry_multiplicity
Co Co1 0.35427(3) 0.50053(6) 0.41073(2) 0.02221(7) Uani d . 1 1
O O11 0.0305(2) 0.2427(3) 0.2280(2) 0.0559(6) Uani d . 1 1
O O21 0.15083(17) 0.4560(2) 0.32261(18) 0.0326(4) Uani d . 1 1
O O31 0.39059(19) 0.2551(2) 0.42902(16) 0.0292(4) Uani d . 1 1
O O41 0.44053(15) 0.0217(2) 0.52815(15) 0.0281(4) Uani d . 1 1
C C11 0.1390(2) 0.2443(3) 0.4571(2) 0.0288(5) Uani d . 1 1
C C21 0.0448(3) 0.2621(3) 0.5065(3) 0.0397(6) Uani d . 1 1
H H21 -0.0332 0.3187 0.4587 0.048 Uiso calc R 1 1
C C31 0.0648(3) 0.1978(4) 0.6243(3) 0.0484(8) Uani d . 1 1
H H31 0.0012 0.2125 0.6561 0.058 Uiso calc R 1 1
C C41 0.1780(3) 0.1122(4) 0.6954(3) 0.0481(8) Uani d . 1 1
H H41 0.1920 0.0696 0.7757 0.058 Uiso calc R 1 1
C C51 0.2719(3) 0.0893(4) 0.6464(3) 0.0399(6) Uani d . 1 1
H H51 0.3469 0.0271 0.6927 0.048 Uiso calc R 1 1
C C61 0.2552(2) 0.1586(3) 0.5287(2) 0.0277(5) Uani d . 1 1
C C71 0.1063(2) 0.3192(3) 0.3255(3) 0.0319(5) Uani d . 1 1
C C81 0.3688(2) 0.1452(3) 0.4906(2) 0.0232(5) Uani d . 1 1
N N12 0.37286(17) 0.5158(3) 0.60643(16) 0.0253(4) Uani d . 1 1
N N22 0.34412(18) 0.4913(4) 1.21618(16) 0.0295(4) Uani d . 1 1
C C12 0.2668(3) 0.5679(4) 0.6219(2) 0.0340(6) Uani d . 1 1
H H12 0.1949 0.6083 0.5493 0.041 Uiso calc R 1 1
C C22 0.2578(3) 0.5651(3) 0.7385(2) 0.0347(6) Uani d . 1 1
H H22 0.1814 0.6027 0.7437 0.042 Uiso calc R 1 1
C C32 0.3635(2) 0.5059(4) 0.84854(19) 0.0268(4) Uani d . 1 1
C C42 0.4757(3) 0.4573(3) 0.8339(2) 0.0346(6) Uani d . 1 1
H H42 0.5505 0.4203 0.9054 0.041 Uiso calc R 1 1
C C52 0.4761(2) 0.4637(3) 0.7132(2) 0.0318(6) Uani d . 1 1
H H52 0.5523 0.4300 0.7057 0.038 Uiso calc R 1 1
C C62 0.2767(3) 0.5978(4) 1.1257(2) 0.0403(7) Uani d . 1 1
H H62 0.2239 0.6707 1.1438 0.048 Uiso calc R 1 1
C C72 0.2803(3) 0.6066(4) 1.0062(3) 0.0414(7) Uani d . 1 1
H H72 0.2326 0.6852 0.9468 0.050 Uiso calc R 1 1
C C82 0.3556(2) 0.4975(4) 0.97543(19) 0.0280(4) Uani d . 1 1
C C92 0.4228(3) 0.3828(3) 1.0675(2) 0.0369(6) Uani d . 1 1
H H92 0.4732 0.3057 1.0503 0.044 Uiso calc R 1 1
C C102 0.4148(3) 0.3834(3) 1.1853(2) 0.0367(6) Uani d . 1 1
H H102 0.4607 0.3053 1.2462 0.044 Uiso calc R 1 1
O O1W 0.30884(19) 0.74617(19) 0.39430(17) 0.0359(4) Uani d D 1 1
H H1WA 0.3694(9) 0.8086(14) 0.4445(19) 0.043 Uiso d D 1 1
H H1WB 0.2452(8) 0.8072(13) 0.3472(15) 0.043 Uiso d D 1 1
O O2W 0.1079(2) 0.9216(3) 0.2094(3) 0.0914(10) Uani d D 1 1
H H2WA 0.1460(8) 0.947(2) 0.1613(9) 0.110 Uiso d D 1 1
H H2WB 0.0868(16) 1.0100(13) 0.232(2) 0.110 Uiso d D 1 1
O O3W 0.1274(5) 0.9518(4) -0.0226(3) 0.132(2) Uani d PD 0.80 1
H H3WA 0.0890(15) 0.8997(18) -0.0931(9) 0.159 Uiso d D 0.80 1
H H3WB 0.093(2) 1.0440(12) -0.041(3) 0.159 Uiso d D 0.80 1
O O4W -0.0925(4) 0.7527(6) 0.0073(3) 0.124(2) Uani d PD 0.70 1
H H4WB -0.0722(18) 0.788(4) -0.0518(11) 0.149 Uiso d D 0.70 1
H H4WA -0.0434(19) 0.8035(15) 0.0761(8) 0.149 Uiso d D 0.70 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.3490 0.9720 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 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
O21 Co1 O41 . 2_656 169.71(7)
O21 Co1 O31 . . 89.59(7)
O41 Co1 O31 2_656 . 85.12(7)
O21 Co1 O1W . . 88.01(7)
O41 Co1 O1W 2_656 . 97.52(7)
O31 Co1 O1W . . 177.00(8)
O21 Co1 N12 . . 96.29(7)
O41 Co1 N12 2_656 . 92.68(6)
O31 Co1 N12 . . 91.59(8)
O1W Co1 N12 . . 86.89(8)
O21 Co1 N22 . 1_554 86.21(7)
O41 Co1 N22 2_656 1_554 84.92(7)
O31 Co1 N22 . 1_554 89.38(9)
O1W Co1 N22 . 1_554 92.25(9)
N12 Co1 N22 . 1_554 177.33(9)
C71 O21 Co1 . . 120.77(16)
C81 O31 Co1 . . 135.33(16)
C81 O41 Co1 . 2_646 128.39(15)
C21 C11 C61 . . 119.1(2)
C21 C11 C71 . . 116.8(2)
C61 C11 C71 . . 124.0(2)
C31 C21 C11 . . 121.2(3)
C31 C21 H21 . . 119.4
C11 C21 H21 . . 119.4
C41 C31 C21 . . 120.3(3)
C41 C31 H31 . . 119.8
C21 C31 H31 . . 119.8
C31 C41 C51 . . 119.5(3)
C31 C41 H41 . . 120.3
C51 C41 H41 . . 120.3
C41 C51 C61 . . 120.9(3)
C41 C51 H51 . . 119.6
C61 C51 H51 . . 119.6
C11 C61 C51 . . 118.9(2)
C11 C61 C81 . . 123.4(2)
C51 C61 C81 . . 117.6(2)
O11 C71 O21 . . 124.8(3)
O11 C71 C11 . . 116.6(2)
O21 C71 C11 . . 118.4(2)
O31 C81 O41 . . 123.5(2)
O31 C81 C61 . . 119.8(2)
O41 C81 C61 . . 116.6(2)
C52 N12 C12 . . 116.54(19)
C52 N12 Co1 . . 125.78(15)
C12 N12 Co1 . . 117.34(15)
C62 N22 C102 . . 116.84(19)
C62 N22 Co1 . 1_556 122.12(19)
C102 N22 Co1 . 1_556 120.85(17)
N12 C12 C22 . . 123.9(2)
N12 C12 H12 . . 118.1
C22 C12 H12 . . 118.1
C12 C22 C32 . . 119.4(2)
C12 C22 H22 . . 120.3
C32 C22 H22 . . 120.3
C22 C32 C42 . . 116.8(2)
C22 C32 C82 . . 120.8(2)
C42 C32 C82 . . 122.4(2)
C52 C42 C32 . . 119.9(2)
C52 C42 H42 . . 120.1
C32 C42 H42 . . 120.1
N12 C52 C42 . . 123.4(2)
N12 C52 H52 . . 118.3
C42 C52 H52 . . 118.3
N22 C62 C72 . . 123.7(2)
N22 C62 H62 . . 118.2
C72 C62 H62 . . 118.2
C62 C72 C82 . . 119.4(2)
C62 C72 H72 . . 120.3
C82 C72 H72 . . 120.3
C92 C82 C72 . . 117.3(2)
C92 C82 C32 . . 122.1(2)
C72 C82 C32 . . 120.6(2)
C102 C92 C82 . . 119.6(2)
C102 C92 H92 . . 120.2
C82 C92 H92 . . 120.2
N22 C102 C92 . . 123.1(2)
N22 C102 H102 . . 118.4
C92 C102 H102 . . 118.4
Co1 O1W H1WA . . 117.0(9)
Co1 O1W H1WB . . 138.3(10)
H1WA O1W H1WB . . 104.6(9)
H2WA O2W H2WB . . 104.6(11)
H3WA O3W H3WB . . 104.3(11)
H4WB O4W H4WA . . 105.5(11)
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 O21 . 2.0710(18) y
Co1 O41 2_656 2.0819(16) y
Co1 O31 . 2.0947(18) y
Co1 O1W . 2.1141(17) y
Co1 N12 . 2.1486(17) y
Co1 N22 1_554 2.1678(17) y
O11 C71 . 1.244(3) ?
O21 C71 . 1.257(3) ?
O31 C81 . 1.244(3) ?
O41 C81 . 1.265(3) ?
O41 Co1 2_646 2.0819(16) ?
C11 C21 . 1.392(4) ?
C11 C61 . 1.392(3) ?
C11 C71 . 1.516(4) ?
C21 C31 . 1.371(4) ?
C21 H21 . 0.9300 ?
C31 C41 . 1.368(5) ?
C31 H31 . 0.9300 ?
C41 C51 . 1.391(4) ?
C41 H41 . 0.9300 ?
C51 C61 . 1.396(3) ?
C51 H51 . 0.9300 ?
C61 C81 . 1.504(3) ?
N12 C52 . 1.333(3) ?
N12 C12 . 1.336(3) ?
N22 C62 . 1.325(4) ?
N22 C102 . 1.341(4) ?
N22 Co1 1_556 2.1678(17) ?
C12 C22 . 1.373(3) ?
C12 H12 . 0.9300 ?
C22 C32 . 1.387(3) ?
C22 H22 . 0.9300 ?
C32 C42 . 1.387(3) ?
C32 C82 . 1.485(3) ?
C42 C52 . 1.375(3) ?
C42 H42 . 0.9300 ?
C52 H52 . 0.9300 ?
C62 C72 . 1.380(4) ?
C62 H62 . 0.9300 ?
C72 C82 . 1.383(4) ?
C72 H72 . 0.9300 ?
C82 C92 . 1.381(4) ?
C92 C102 . 1.380(3) ?
C92 H92 . 0.9300 ?
C102 H102 . 0.9300 ?
O1W H1WA . 0.8501(10) ?
O1W H1WB . 0.8501(10) ?
O2W H2WA . 0.8501(10) ?
O2W H2WB . 0.8500(10) ?
O3W H3WA . 0.8500(10) ?
O3W H3WB . 0.8503(10) ?
O4W H4WB . 0.8500(10) ?
O4W H4WA . 0.8501(10) ?
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
O1W H1WA O41 1_565 0.850(16) 2.022(14) 2.810(2) 153.9(13)
O1W H1WB O2W . 0.850(13) 1.908(14) 2.743(3) 166.8(14)
O2W H2WA O3W . 0.850(11) 2.012(10) 2.751(5) 144.8(10)
O2W H2WB O11 1_565 0.851(14) 2.048(12) 2.867(4) 161.4(19)
O3W H3WA O11 2_555 0.849(12) 2.024(13) 2.843(4) 161.7(15)
O3W H3WB O4W 2_555 0.849(15) 1.796(13) 2.576(6) 152.1(19)
O4W H4WB O11 2_555 0.850(19) 2.275(16) 3.038(4) 150.0(19)
O4W H4WA O2W . 0.851(11) 1.976(14) 2.799(5) 162.3(18)
