#------------------------------------------------------------------------------
#$Date: 2019-12-26 22:31:21 +0200 (Thu, 26 Dec 2019) $
#$Revision: 246195 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/19/2311974.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_2311974
loop_
_publ_author_name
'Atria, Ana María'
'Parada, José'
'Moreno, Yanko'
'Suárez, Sebastián'
'Baggio, Ricardo'
'Peña, Octavio'
_publ_section_title
;
 Synthesis, crystal structure and magnetic properties of
 diaquabis(2,6-diamino-7H-purin-1-ium-\kN⁹)bis(4,4'-oxydibenzoato-\kO)cobalt(II)
 dihydrate.
;
_journal_coeditor_code           SK3675
_journal_issue                   'Pt 1'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              37
_journal_page_last               44
_journal_paper_doi               10.1107/S2053229617016916
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac
'[Co (C5 H7 N6)2 (C14 H8 O5)2 (H2 O)2], 2H2 O'
_chemical_formula_moiety         'C38 H34 Co N12 O12, 2(H2 O)'
_chemical_formula_sum            'C38 H38 Co N12 O14'
_chemical_formula_weight         945.73
_chemical_name_systematic
'Diaquabis(2,6-diamino-7H-purin-1-ium-κN⁹)bis(4,4'-oxydibenzoato-κO)cobalt(II) dihydrate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                73.757(2)
_cell_angle_beta                 88.232(2)
_cell_angle_gamma                83.876(2)
_cell_formula_units_Z            1
_cell_length_a                   7.3560(9)
_cell_length_b                   11.5890(15)
_cell_length_c                   12.0655(15)
_cell_measurement_reflns_used    4255
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.78
_cell_volume                     981.9(2)
_computing_cell_refinement
;
SAINT (Bruker, 2002)
;
_computing_data_collection
;
SMART (Bruker, 2001)
;
_computing_data_reduction
;
SAINT (Bruker, 2002)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0135
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8230
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.769
_diffrn_reflns_theta_min         1.758
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2008)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       block
_exptl_crystal_F_000             489
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4207
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0446P)²+0.4856P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0869
_reflns_number_gt                3861
_reflns_number_total             4207
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            sk3675sup1.cif
_cod_data_source_block           I
_cod_database_code               2311974
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_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_occupancy
Co Co1 0.500000 0.500000 0.500000 0.01676(9) Uani d 1
N N11 0.47146(18) 0.62667(12) 0.33268(11) 0.0207(3) Uani d 1
N N21 0.44483(19) 0.81452(12) 0.21500(12) 0.0220(3) Uani d 1
H H21 0.452(3) 0.8907(19) 0.1941(17) 0.026 Uiso d 1
N N31 0.33331(19) 0.77944(12) 0.04178(12) 0.0232(3) Uani d 1
N N41 0.2233(2) 0.70938(15) -0.10148(14) 0.0326(4) Uani d 1
H H41A 0.216(3) 0.783(2) -0.145(2) 0.039 Uiso d 1
H H41B 0.186(3) 0.650(2) -0.1236(19) 0.039 Uiso d 1
N N51 0.30455(19) 0.56951(12) 0.06912(12) 0.0219(3) Uani d 1
H H51 0.254(4) 0.503(3) 0.020(3) 0.086(10) Uiso d 1
N N61 0.3814(2) 0.41629(13) 0.23437(13) 0.0238(3) Uani d 1
H H61A 0.358(3) 0.3686(19) 0.1978(18) 0.029 Uiso d 1
H H61B 0.442(3) 0.3890(18) 0.2970(18) 0.029 Uiso d 1
C C11 0.4892(2) 0.74191(14) 0.32141(14) 0.0226(3) Uani d 1
H H11 0.529165 0.770647 0.382028 0.027 Uiso calc 1
C C21 0.3935(2) 0.74306(14) 0.15154(14) 0.0198(3) Uani d 1
C C31 0.2889(2) 0.68775(15) 0.00598(14) 0.0232(3) Uani d 1
C C41 0.3682(2) 0.53356(14) 0.17898(14) 0.0200(3) Uani d 1
C C51 0.4125(2) 0.62581(14) 0.22460(13) 0.0188(3) Uani d 1
O O12 0.37407(15) 0.63681(10) 0.57105(9) 0.0204(2) Uani d 1
O O22 0.08856(16) 0.58410(10) 0.59471(11) 0.0248(3) Uani d 1
O O32 0.2025(2) 1.44220(11) 0.94800(11) 0.0336(3) Uani d 1
O O42 0.26406(17) 1.27054(11) 1.08592(10) 0.0278(3) Uani d 1
O O52 -0.05963(17) 1.10192(11) 0.67491(11) 0.0285(3) Uani d 1
C C12 0.2043(2) 0.65636(14) 0.59254(13) 0.0186(3) Uani d 1
C C22 0.1403(2) 0.77421(14) 0.61705(13) 0.0191(3) Uani d 1
C C32 0.2609(2) 0.85769(15) 0.62081(14) 0.0232(3) Uani d 1
H H32 0.387501 0.840318 0.607484 0.028 Uiso calc 1
C C42 0.1987(2) 0.96598(15) 0.64375(15) 0.0257(4) Uani d 1
H H42 0.282249 1.021996 0.647249 0.031 Uiso calc 1
C C52 0.0134(2) 0.99162(14) 0.66152(14) 0.0224(3) Uani d 1
C C62 -0.1086(2) 0.91020(16) 0.65789(16) 0.0268(4) Uani d 1
H H62 -0.235331 0.928434 0.670017 0.032 Uiso calc 1
C C72 -0.0448(2) 0.80172(15) 0.63645(15) 0.0254(4) Uani d 1
H H72 -0.128535 0.745188 0.634942 0.030 Uiso calc 1
C C82 0.2096(2) 1.32678(14) 0.98709(14) 0.0222(3) Uani d 1
C C92 0.1460(2) 1.26402(14) 0.90480(14) 0.0202(3) Uani d 1
C C102 0.1499(2) 1.13827(14) 0.93475(14) 0.0224(3) Uani d 1
H H102 0.195580 1.091393 1.008128 0.027 Uiso calc 1
C C112 0.0878(2) 1.08120(14) 0.85872(14) 0.0233(3) Uani d 1
H H112 0.091338 0.995647 0.879333 0.028 Uiso calc 1
C C122 0.0204(2) 1.15077(15) 0.75180(14) 0.0212(3) Uani d 1
C C132 0.0164(2) 1.27536(15) 0.71998(14) 0.0227(3) Uani d 1
H H132 -0.029135 1.321958 0.646447 0.027 Uiso calc 1
C C142 0.0795(2) 1.33135(14) 0.79673(14) 0.0221(3) Uani d 1
H H142 0.077402 1.416850 0.775266 0.026 Uiso calc 1
O O1W 0.25220(16) 0.42894(11) 0.49195(11) 0.0237(3) Uani d 1
H H1WA 0.187(3) 0.4249(19) 0.440(2) 0.036 Uiso d 1
H H1WB 0.187(3) 0.470(2) 0.5279(19) 0.036 Uiso d 1
O O2W 0.48410(19) 1.05787(11) 1.14845(12) 0.0288(3) Uani d 1
H H2WA 0.396(3) 1.118(2) 1.135(2) 0.043 Uiso d 1
H H2WB 0.555(3) 1.081(2) 1.094(2) 0.043 Uiso d 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
O1W Co1 N11 . . 94.58(5) y
O12 Co1 N11 . . 88.49(5) y
O1W Co1 O12 . . 92.75(5) y
O1W Co1 O12 . 2_666 87.25(5) y
O12 Co1 N11 . 2_666 91.51(5) y
O1W Co1 N11 . 2_666 85.42(5) y
O1W Co1 O12 2_666 . 87.25(5) ?
O1W Co1 N11 2_666 . 85.42(5) ?
O12 Co1 N11 2_666 . 91.51(5) ?
N11 Co1 N11 2_666 . 180.0 ?
O1W Co1 O1W 2_666 . 180.0 ?
O12 Co1 O12 2_666 . 180.0 ?
O1W Co1 O12 2_666 2_666 92.75(5) ?
O1W Co1 N11 2_666 2_666 94.58(5) ?
O12 Co1 N11 2_666 2_666 88.49(5) ?
C11 N11 C51 . . 103.98(13) ?
C11 N11 Co1 . . 119.17(11) ?
C51 N11 Co1 . . 136.22(11) ?
C11 N21 C21 . . 107.21(13) ?
C11 N21 H21 . . 124.1(13) ?
C21 N21 H21 . . 128.7(13) ?
C31 N31 C21 . . 111.90(14) ?
C31 N41 H41A . . 118.0(15) ?
C31 N41 H41B . . 119.4(15) ?
H41A N41 H41B . . 123(2) ?
C41 N51 C31 . . 122.03(14) ?
C41 N51 H51 . . 124.1(15) ?
C31 N51 H51 . . 113.8(15) ?
C41 N61 H61A . . 117.9(14) ?
C41 N61 H61B . . 120.4(14) ?
H61A N61 H61B . . 119(2) ?
N11 C11 N21 . . 113.22(14) ?
N11 C11 H11 . . 123.4 ?
N21 C11 H11 . . 123.4 ?
N31 C21 N21 . . 126.75(14) ?
N31 C21 C51 . . 127.53(15) ?
N21 C21 C51 . . 105.71(14) ?
N31 C31 N41 . . 119.25(16) ?
N31 C31 N51 . . 125.61(15) ?
N41 C31 N51 . . 115.14(15) ?
N61 C41 N51 . . 118.37(15) ?
N61 C41 C51 . . 125.76(15) ?
N51 C41 C51 . . 115.87(14) ?
N11 C51 C21 . . 109.87(14) ?
N11 C51 C41 . . 133.10(15) ?
C21 C51 C41 . . 117.02(15) ?
C12 O12 Co1 . . 127.06(10) ?
C52 O52 C122 . . 119.67(12) ?
O22 C12 O12 . . 124.47(14) ?
O22 C12 C22 . . 118.11(14) ?
O12 C12 C22 . . 117.42(14) ?
C32 C22 C72 . . 118.60(14) ?
C32 C22 C12 . . 121.86(14) ?
C72 C22 C12 . . 119.54(14) ?
C42 C32 C22 . . 120.87(15) ?
C42 C32 H32 . . 119.6 ?
C22 C32 H32 . . 119.6 ?
C32 C42 C52 . . 119.31(15) ?
C32 C42 H42 . . 120.3 ?
C52 C42 H42 . . 120.3 ?
C62 C52 O52 . . 116.86(15) ?
C62 C52 C42 . . 120.73(15) ?
O52 C52 C42 . . 122.24(15) ?
C52 C62 C72 . . 119.49(16) ?
C52 C62 H62 . . 120.3 ?
C72 C62 H62 . . 120.3 ?
C62 C72 C22 . . 120.99(16) ?
C62 C72 H72 . . 119.5 ?
C22 C72 H72 . . 119.5 ?
O42 C82 O32 . . 123.02(15) ?
O42 C82 C92 . . 122.04(15) ?
O32 C82 C92 . . 114.94(14) ?
C142 C92 C102 . . 118.91(15) ?
C142 C92 C82 . . 119.87(14) ?
C102 C92 C82 . . 121.21(14) ?
C112 C102 C92 . . 120.77(15) ?
C112 C102 H102 . . 119.6 ?
C92 C102 H102 . . 119.6 ?
C102 C112 C122 . . 119.11(15) ?
C102 C112 H112 . . 120.4 ?
C122 C112 H112 . . 120.4 ?
C132 C122 O52 . . 115.90(14) ?
C132 C122 C112 . . 121.13(15) ?
O52 C122 C112 . . 122.77(15) ?
C122 C132 C142 . . 119.18(15) ?
C122 C132 H132 . . 120.4 ?
C142 C132 H132 . . 120.4 ?
C132 C142 C92 . . 120.90(15) ?
C132 C142 H142 . . 119.5 ?
C92 C142 H142 . . 119.5 ?
Co1 O1W H1WA . . 135.0(16) ?
Co1 O1W H1WB . . 98.3(15) ?
H1WA O1W H1WB . . 105(2) ?
H2WA O2W H2WB . . 102(2) ?
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 O1W 2_666 2.0943(12) ?
Co1 O1W . 2.0943(12) y
Co1 O12 2_666 2.1224(11) ?
Co1 O12 . 2.1224(11) y
Co1 N11 2_666 2.1394(13) ?
Co1 N11 . 2.1394(13) y
N11 C11 . 1.324(2) ?
N11 C51 . 1.390(2) ?
N21 C11 . 1.351(2) ?
N21 C21 . 1.361(2) ?
N21 H21 . 0.85(2) ?
N31 C31 . 1.327(2) ?
N31 C21 . 1.346(2) ?
N41 C31 . 1.345(2) ?
N41 H41A . 0.86(2) ?
N41 H41B . 0.88(2) ?
N51 C41 . 1.355(2) ?
N51 C31 . 1.363(2) ?
N51 H51 . 1.19(3) ?
N61 C41 . 1.331(2) ?
N61 H61A . 0.83(2) ?
N61 H61B . 0.85(2) ?
C11 H11 . 0.9500 ?
C21 C51 . 1.393(2) ?
C41 C51 . 1.402(2) ?
O12 C12 . 1.2773(19) ?
O22 C12 . 1.2509(19) ?
O32 C82 . 1.284(2) ?
O42 C82 . 1.244(2) ?
O52 C52 . 1.3828(19) ?
O52 C122 . 1.3878(19) ?
C12 C22 . 1.502(2) ?
C22 C32 . 1.391(2) ?
C22 C72 . 1.392(2) ?
C32 C42 . 1.387(2) ?
C32 H32 . 0.9500 ?
C42 C52 . 1.387(2) ?
C42 H42 . 0.9500 ?
C52 C62 . 1.379(2) ?
C62 C72 . 1.384(2) ?
C62 H62 . 0.9500 ?
C72 H72 . 0.9500 ?
C82 C92 . 1.496(2) ?
C92 C142 . 1.392(2) ?
C92 C102 . 1.397(2) ?
C102 C112 . 1.384(2) ?
C102 H102 . 0.9500 ?
C112 C122 . 1.390(2) ?
C112 H112 . 0.9500 ?
C122 C132 . 1.384(2) ?
C132 C142 . 1.386(2) ?
C132 H132 . 0.9500 ?
C142 H142 . 0.9500 ?
O1W H1WA . 0.81(2) ?
O1W H1WB . 0.84(2) ?
O2W H2WA . 0.88(2) ?
O2W H2WB . 0.83(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
_geom_hbond_publ_flag
O1W H1WB O22 . 0.84(2) 1.81(2) 2.6291(17) 166(2) no
O2W H2WA O42 . 0.88(2) 1.87(3) 2.7290(18) 164(2) no
N61 H61B O12 2_666 0.85(2) 2.06(2) 2.8885(19) 164.6(19) no
N41 H41B O32 1_544 0.88(2) 2.31(2) 3.005(2) 136.3(19) no
N51 H51 O32 1_544 1.19(3) 1.35(3) 2.5272(18) 171(3) no
N61 H61A O42 1_544 0.83(2) 2.16(2) 2.9840(19) 169.9(19) no
N21 H21 O2W 1_554 0.85(2) 1.90(2) 2.7522(19) 176.3(19) no
O1W H1WA O22 2_566 0.81(2) 2.10(2) 2.7803(17) 141(2) no
O2W H2WB N31 2_676 0.83(3) 2.16(3) 2.9251(19) 152(2) no
