#------------------------------------------------------------------------------
#$Date: 2017-09-25 15:16:39 +0200 (lun 25 de sep de 2017) $
#$Revision: 201255 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/92/7229241.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7229241
loop_
_publ_author_name
'Jiang, Wen-Hong'
'Zhang, Han-Zhong'
'Hou, Guang-Feng'
'Ma, Dong-Sheng'
'Liu, Bin'
'Yu, Ying-Hui'
_publ_section_title
;
 Five Co(ii) coordination polymers with different counter anions based on
 [3,5-di(4H-1,2,4-triazol-4-yl)benzoato]− ligand: directed
 synthesis, structures and magnetic properties
;
_journal_issue                   72
_journal_name_full               'RSC Adv.'
_journal_page_first              45641
_journal_paper_doi               10.1039/C7RA07089F
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         '[Co2 (H2 O) (O4 S) (C11 H7 N6 O2)2], 2H2 O'
_chemical_formula_sum            'C22 H20 Co2 N12 O11 S'
_chemical_formula_weight         778.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           25
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 -2'
_symmetry_space_group_name_H-M   'P m m 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-01-17 deposited with the CCDC.
2017-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   6.9023(2)
_cell_length_b                   11.6321(4)
_cell_length_c                   8.0322(3)
_cell_measurement_reflns_used    951
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.0620
_cell_measurement_theta_min      3.4240
_cell_volume                     644.89(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_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  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1826
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    1.459
_exptl_absorpt_correction_T_max  0.8218
_exptl_absorpt_correction_T_min  0.7209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis PRO (Agilent, 2014)'
_exptl_crystal_colour            reddish-brown
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             394
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 'Flack parameter from 246 Friedel pairs'
_refine_ls_abs_structure_Flack   0.32(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         1114
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0359P)²+0.2577P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                1031
_reflns_number_total             1114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ra07089f2.cif
_cod_data_source_block           5-Co
_cod_database_code               7229241
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, z'
'x, -y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Co1 Co 0.74455(10) 0.5000 0.49998(16) 0.0112(2) Uani 0.976(4) 2 d SP .
S1 S 0.5000 0.5000 0.1435(3) 0.0197(5) Uani 1 4 d SD .
O1 O 1.0000 1.0971(4) -0.3297(6) 0.0248(11) Uani 1 2 d S .
O2 O 0.5000 -0.0967(4) 1.3529(6) 0.0262(11) Uani 1 2 d S .
O3 O 0.5000 0.5000 0.3332(6) 0.0206(14) Uani 1 4 d SD 1
O4 O 0.4178(17) 0.3867(9) 0.0949(15) 0.0357(17) Uani 0.25 1 d PD 1
O5 O 0.7038(9) 0.5000 0.0913(10) 0.0357(17) Uani 0.50 2 d SPD 1
O6 O 0.3885(16) 0.5929(10) 0.0800(14) 0.0357(17) Uani 0.25 1 d PD 1
O1w O 1.0000 0.5000 0.6744(7) 0.0156(13) Uani 1 4 d S .
H1w H 1.0000 0.4412 0.7350 0.023 Uiso 1 2 d SR .
O2w O 1.0000 0.3707(4) 0.9466(6) 0.0402(13) Uani 1 2 d S .
H2w H 0.9015 0.4043 0.9840 0.060 Uiso 1 1 d R .
N1 N 0.8988(4) 0.6329(3) 0.3884(5) 0.0162(8) Uani 1 1 d . .
N2 N 1.0000 0.7912(4) 0.2773(6) 0.0131(10) Uani 1 2 d S .
N3 N 0.5989(4) 0.3693(3) 0.6342(5) 0.0154(8) Uani 1 1 d . .
N4 N 0.5000 0.2096(4) 0.7478(6) 0.0142(10) Uani 1 2 d S .
C1 C 0.8452(5) 0.7299(3) 0.3232(5) 0.0189(10) Uani 1 1 d . .
H1 H 0.7173 0.7534 0.3102 0.023 Uiso 1 1 calc R .
C2 C 1.0000 1.0000 0.2827(12) 0.013(2) Uani 1 4 d S .
H2 H 1.0000 1.0000 0.3984 0.016 Uiso 1 4 calc SR .
C3 C 1.0000 0.9006(5) 0.1909(7) 0.0128(13) Uani 1 2 d S .
C4 C 1.0000 0.8981(5) 0.0173(8) 0.0151(14) Uani 1 2 d S .
H4 H 1.0000 0.8280 -0.0385 0.018 Uiso 1 2 calc SR .
C5 C 1.0000 1.0000 -0.0720(10) 0.0131(18) Uani 1 4 d S .
C6 C 1.0000 1.0000 -0.2572(13) 0.015(2) Uani 1 4 d S .
C7 C 0.6551(6) 0.2722(4) 0.7031(6) 0.0206(10) Uani 1 1 d . .
H7 H 0.7834 0.2502 0.7186 0.025 Uiso 1 1 calc R .
C8 C 0.5000 0.0000 0.7448(12) 0.015(2) Uani 1 4 d S .
H8 H 0.5000 0.0000 0.6291 0.018 Uiso 1 4 calc SR .
C9 C 0.5000 0.1009(4) 0.8372(8) 0.0130(12) Uani 1 2 d S .
C10 C 0.5000 0.1025(5) 1.0056(9) 0.0141(11) Uani 1 2 d S .
H10 H 0.5000 0.1723 1.0619 0.017 Uiso 1 2 calc SR .
C11 C 0.5000 0.0000 1.0950(11) 0.016(2) Uani 1 4 d S .
C12 C 0.5000 0.0000 1.2870(13) 0.015(2) Uani 1 4 d S .
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'
S S 0.1246 0.1234 '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_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Co1 N1 96.02(19) 4_565 .
N1 Co1 N3 85.92(11) 4_565 .
N1 Co1 N3 174.82(18) . .
N1 Co1 N3 174.82(18) 4_565 4_565
N1 Co1 N3 85.92(11) . 4_565
N3 Co1 N3 91.75(18) . 4_565
N1 Co1 O3 97.65(12) 4_565 .
N1 Co1 O3 97.65(12) . .
N3 Co1 O3 86.82(12) . .
N3 Co1 O3 86.82(12) 4_565 .
N1 Co1 O1w 82.37(12) 4_565 .
N1 Co1 O1w 82.37(12) . .
N3 Co1 O1w 93.15(13) . .
N3 Co1 O1w 93.15(13) 4_565 .
O3 Co1 O1w 179.97(19) . .
O6 S1 O5 114.6(5) . .
O6 S1 O4 111.9(5) . .
O5 S1 O4 106.9(5) . .
O6 S1 O3 111.1(5) . .
O5 S1 O3 106.6(3) . .
O4 S1 O3 105.2(5) . .
S1 O3 Co1 128.44(10) . .
Co1 O1w Co1 103.1(2) 2_765 .
Co1 O1w H1w 111.1 2_765 .
Co1 O1w H1w 111.1 . .
C1 N1 N1 106.6(2) . 3_755
C1 N1 Co1 132.4(3) . .
N1 N1 Co1 120.79(9) 3_755 .
C1 N2 C1 106.2(4) 3_755 .
C1 N2 C3 126.9(2) 3_755 .
C1 N2 C3 126.9(2) . .
C7 N3 N3 107.2(2) . 3_655
C7 N3 Co1 133.6(3) . .
N3 N3 Co1 118.35(9) 3_655 .
C7 N4 C7 105.6(5) 3_655 .
C7 N4 C9 127.1(2) 3_655 .
C7 N4 C9 127.1(2) . .
N1 C1 N2 110.3(3) . .
N1 C1 H1 124.9 . .
N2 C1 H1 124.9 . .
C3 C2 C3 115.0(9) 2_775 .
C3 C2 H2 122.5 2_775 .
C3 C2 H2 122.5 . .
C2 C3 C4 123.7(6) . .
C2 C3 N2 118.9(5) . .
C4 C3 N2 117.4(5) . .
C5 C4 C3 120.0(6) . .
C5 C4 H4 120.0 . .
C3 C4 H4 120.0 . .
C4 C5 C4 117.6(8) 2_775 .
C4 C5 C6 121.2(4) 2_775 .
C4 C5 C6 121.2(4) . .
O1 C6 O1 125.4(9) . 2_775
O1 C6 C5 117.3(5) . .
O1 C6 C5 117.3(5) 2_775 .
N3 C7 N4 110.0(4) . .
N3 C7 H7 125.0 . .
N4 C7 H7 125.0 . .
C9 C8 C9 115.4(9) 2_655 .
C9 C8 H8 122.3 2_655 .
C9 C8 H8 122.3 . .
C10 C9 C8 123.0(6) . .
C10 C9 N4 118.9(5) . .
C8 C9 N4 118.1(6) . .
C9 C10 C11 120.3(6) . .
C9 C10 H10 119.8 . .
C11 C10 H10 119.8 . .
C10 C11 C10 117.9(9) 2_655 .
C10 C11 C12 121.1(4) 2_655 .
C10 C11 C12 121.1(4) . .
O2 C12 O2 129.6(10) 2_655 .
O2 C12 C11 115.2(5) 2_655 .
O2 C12 C11 115.2(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O3 2.155(3) .
Co1 O1w 2.252(4) .
Co1 N1 2.080(3) .
Co1 N1 2.080(3) 4_565
Co1 N3 2.118(3) .
Co1 N3 2.118(3) 4_565
S1 O6 1.421(7) .
S1 O5 1.468(6) .
S1 O4 1.487(7) .
S1 O3 1.523(5) .
O1 C6 1.271(6) .
O2 C12 1.243(6) .
O3 Co1 2.155(3) 2_665
O4 O6 0.33(3) 4_565
O4 O4 1.13(2) 3_655
O4 O6 1.363(13) 2_665
O4 O5 1.563(14) 2_665
O5 O6 1.257(14) 2_665
O5 O6 1.257(14) 3_655
O5 O4 1.563(14) 3_655
O5 O4 1.563(14) 2_665
O6 O4 0.33(3) 4_565
O6 O5 1.257(14) 2_665
O6 O4 1.363(13) 2_665
O6 O6 1.54(2) 3_655
O1w Co1 2.252(4) 2_765
O1w H1w 0.8401 .
O2w H2w 0.8400 .
N1 C1 1.298(5) .
N1 N1 1.397(6) 3_755
N2 C1 1.336(4) 3_755
N2 C1 1.336(4) .
N2 C3 1.450(7) .
N3 C7 1.316(5) .
N3 N3 1.365(6) 3_655
N4 C7 1.344(5) 3_655
N4 C7 1.344(5) .
N4 C9 1.453(7) .
C1 H1 0.9300 .
C2 C3 1.371(8) 2_775
C2 C3 1.371(8) .
C2 H2 0.9300 .
C3 C4 1.395(9) .
C4 C5 1.386(7) .
C4 H4 0.9300 .
C5 C4 1.386(7) 2_775
C5 C6 1.487(14) .
C6 O1 1.271(6) 2_775
C7 H7 0.9300 .
C8 C9 1.389(7) 2_655
C8 C9 1.389(7) .
C8 H8 0.9300 .
C9 C10 1.352(10) .
C10 C11 1.391(7) .
C10 H10 0.9300 .
C11 C10 1.391(7) 2_655
C11 C12 1.542(14) .
C12 O2 1.243(6) 2_655
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1w H1w O2w 0.84 1.89 2.654(6) 151 .
O2w H2w O5 0.84 1.96 2.792(6) 170 1_556
O2w H2w O6 0.84 2.14 2.919(10) 153 2_666
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O6 S1 O3 Co1 125.5(6) 4_565 .
O6 S1 O3 Co1 -54.5(6) 3_655 .
O6 S1 O3 Co1 54.5(6) 2_665 .
O6 S1 O3 Co1 -125.5(6) . .
O5 S1 O3 Co1 180.0 2_665 .
O5 S1 O3 Co1 0.0 . .
O4 S1 O3 Co1 113.3(5) . .
O4 S1 O3 Co1 -66.7(5) 2_665 .
O4 S1 O3 Co1 66.7(5) 3_655 .
O4 S1 O3 Co1 -113.3(5) 4_565 .
O6 S1 O3 Co1 -54.5(6) 4_565 2_665
O6 S1 O3 Co1 125.5(6) 3_655 2_665
O6 S1 O3 Co1 -125.5(6) 2_665 2_665
O6 S1 O3 Co1 54.5(6) . 2_665
O5 S1 O3 Co1 0.0 2_665 2_665
O5 S1 O3 Co1 180.0 . 2_665
O4 S1 O3 Co1 -66.7(5) . 2_665
O4 S1 O3 Co1 113.3(5) 2_665 2_665
O4 S1 O3 Co1 -113.3(5) 3_655 2_665
O4 S1 O3 Co1 66.7(5) 4_565 2_665
N1 Co1 O3 Co1 131.42(10) 4_565 2_665
N1 Co1 O3 Co1 -131.42(10) . 2_665
N3 Co1 O3 Co1 45.97(9) . 2_665
N3 Co1 O3 Co1 -45.97(9) 4_565 2_665
N1 Co1 O1w Co1 48.58(10) 4_565 2_765
N1 Co1 O1w Co1 -48.58(10) . 2_765
N3 Co1 O1w Co1 134.03(9) . 2_765
N3 Co1 O1w Co1 -134.03(9) 4_565 2_765
O3 Co1 O1w Co1 180(100) . 2_765
N1 Co1 N1 C1 138.2(3) 4_565 .
N3 Co1 N1 C1 -110.1(16) . .
N3 Co1 N1 C1 -46.6(4) 4_565 .
O3 Co1 N1 C1 39.6(4) . .
O1w Co1 N1 C1 -140.4(4) . .
N1 Co1 N1 N1 -48.55(17) 4_565 3_755
N3 Co1 N1 N1 63.2(16) . 3_755
N3 Co1 N1 N1 126.63(10) 4_565 3_755
O3 Co1 N1 N1 -147.14(9) . 3_755
O1w Co1 N1 N1 32.89(11) . 3_755
N1 Co1 N3 C7 39.3(4) 4_565 .
N1 Co1 N3 C7 -72.9(17) . .
N3 Co1 N3 C7 -136.0(4) 4_565 .
O3 Co1 N3 C7 137.2(4) . .
O1w Co1 N3 C7 -42.8(4) . .
N1 Co1 N3 N3 -128.43(10) 4_565 3_655
N1 Co1 N3 N3 119.4(15) . 3_655
N3 Co1 N3 N3 56.20(15) 4_565 3_655
O3 Co1 N3 N3 -30.52(9) . 3_655
O1w Co1 N3 N3 149.46(10) . 3_655
N1 N1 C1 N2 1.5(4) 3_755 .
Co1 N1 C1 N2 175.5(3) . .
C1 N2 C1 N1 -2.5(6) 3_755 .
C3 N2 C1 N1 175.9(5) . .
C3 C2 C3 C4 0.000(4) 2_775 .
C3 C2 C3 N2 180.000(3) 2_775 .
C1 N2 C3 C2 -91.0(5) 3_755 .
C1 N2 C3 C2 91.0(5) . .
C1 N2 C3 C4 89.0(5) 3_755 .
C1 N2 C3 C4 -89.0(5) . .
C2 C3 C4 C5 0.000(3) . .
N2 C3 C4 C5 180.000(2) . .
C3 C4 C5 C4 0.000(4) . 2_775
C3 C4 C5 C6 180.000(3) . .
C4 C5 C6 O1 0.000(3) 2_775 .
C4 C5 C6 O1 180.000(2) . .
C4 C5 C6 O1 180.000(2) 2_775 2_775
C4 C5 C6 O1 0.000(3) . 2_775
N3 N3 C7 N4 -0.1(4) 3_655 .
Co1 N3 C7 N4 -168.8(3) . .
C7 N4 C7 N3 0.1(7) 3_655 .
C9 N4 C7 N3 -175.6(5) . .
C9 C8 C9 C10 0.000(2) 2_655 .
C9 C8 C9 N4 180.000(1) 2_655 .
C7 N4 C9 C10 -87.5(5) 3_655 .
C7 N4 C9 C10 87.5(5) . .
C7 N4 C9 C8 92.5(5) 3_655 .
C7 N4 C9 C8 -92.5(5) . .
C8 C9 C10 C11 0.000(3) . .
N4 C9 C10 C11 180.000(2) . .
C9 C10 C11 C10 0.000(3) . 2_655
C9 C10 C11 C12 180.000(3) . .
C10 C11 C12 O2 180.000(2) 2_655 2_655
C10 C11 C12 O2 0.000(3) . 2_655
C10 C11 C12 O2 0.000(3) 2_655 .
C10 C11 C12 O2 180.000(2) . .
