#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:03:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180024 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/18/7031826.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_7031826
loop_
_publ_author_name
'Wang, Kangcai'
'Luo, Daibing'
'Xu, Dingguo'
'Guo, Furong'
'Liu, Lin'
'Lin, Zhien'
_publ_section_title
;
 New open-framework cobalt sulfate-oxalates based on molecular and
 chain-like building blocks.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13476
_journal_page_last               13479
_journal_paper_doi               10.1039/c4dt01503g
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C7 H18 Co2 N3 O12 S'
_chemical_formula_weight         486.16
_chemical_name_systematic
; 
 ? 
;
_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                77.884(4)
_cell_angle_beta                 82.744(4)
_cell_angle_gamma                87.356(4)
_cell_formula_units_Z            2
_cell_length_a                   8.6065(3)
_cell_length_b                   9.5595(5)
_cell_length_c                   9.5987(5)
_cell_measurement_reflns_used    3415
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6590
_cell_measurement_theta_min      3.4210
_cell_volume                     765.79(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_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  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5782
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.20
_exptl_absorpt_coefficient_mu    2.375
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.108
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             494
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         2696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0266
_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)+(0.0266P)²+0.2782P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0638
_reflns_number_gt                2374
_reflns_number_total             2696
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01503g2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7031826--7031827.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7031826
loop_
_symmetry_equiv_pos_as_xyz
'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
Co1 Co 0.34974(4) 0.09000(4) 0.23608(4) 0.01735(11) Uani 1 1 d .
Co2 Co 0.5000 0.5000 0.5000 0.01959(14) Uani 1 2 d S
Co3 Co 0.0000 0.5000 0.0000 0.01964(14) Uani 1 2 d S
S1 S 0.02013(7) 0.26796(7) 0.33143(7) 0.01587(15) Uani 1 1 d .
O1 O 0.1219(2) 0.1821(2) 0.2451(2) 0.0283(5) Uani 1 1 d .
O2 O -0.0350(2) 0.3958(2) 0.2366(2) 0.0326(5) Uani 1 1 d .
O3 O -0.1138(3) 0.1808(2) 0.4028(2) 0.0434(6) Uani 1 1 d .
O4 O 0.1048(2) 0.3092(2) 0.4396(2) 0.0282(5) Uani 1 1 d .
O5 O 0.5263(2) 0.4581(2) 0.29341(19) 0.0258(5) Uani 1 1 d .
O6 O 0.4576(2) 0.2897(2) 0.18403(19) 0.0258(5) Uani 1 1 d .
O7 O 0.4632(2) 0.27884(19) 0.54952(19) 0.0218(4) Uani 1 1 d .
O8 O 0.3956(2) 0.11277(19) 0.43728(19) 0.0216(4) Uani 1 1 d .
O9 O 0.5633(2) -0.0135(2) 0.16782(18) 0.0214(4) Uani 1 1 d .
O10 O 0.6801(2) -0.0879(2) -0.02615(19) 0.0231(4) Uani 1 1 d .
OW1 O 0.2798(2) -0.11984(19) 0.32748(19) 0.0237(4) Uani 1 1 d .
H1 H 0.2192 -0.1339 0.4054 0.036 Uiso 1 1 d R
H2 H 0.3611 -0.1708 0.3449 0.036 Uiso 1 1 d R
OW2 O 0.2588(2) 0.5340(2) 0.4949(2) 0.0362(5) Uani 1 1 d .
H3 H 0.2087 0.5580 0.5676 0.054 Uiso 1 1 d R
H4 H 0.2042 0.4722 0.4732 0.054 Uiso 1 1 d R
N2 N 0.0116(2) 0.7117(2) 0.0435(2) 0.0200(5) Uani 1 1 d .
H5 H -0.0354 0.7728 -0.0256 0.024 Uiso 1 1 calc R
N3 N -0.1661(2) 0.9153(2) 0.3240(2) 0.0222(5) Uani 1 1 d .
H6 H -0.1639 1.0069 0.3297 0.033 Uiso 1 1 calc R
H7 H -0.1328 0.8607 0.4020 0.033 Uiso 1 1 calc R
H8 H -0.2637 0.8925 0.3177 0.033 Uiso 1 1 calc R
N1 N 0.2427(3) 0.4981(3) 0.0038(2) 0.0255(5) Uani 1 1 d .
H9 H 0.2755 0.4129 0.0520 0.031 Uiso 1 1 calc R
H10 H 0.2927 0.5139 -0.0861 0.031 Uiso 1 1 calc R
C1 C 0.4785(3) 0.3364(3) 0.2929(3) 0.0194(6) Uani 1 1 d .
C2 C 0.4428(3) 0.2329(3) 0.4387(3) 0.0174(6) Uani 1 1 d .
C3 C 0.5701(3) -0.0296(3) 0.0416(3) 0.0169(6) Uani 1 1 d .
C4 C 0.2749(3) 0.6134(3) 0.0766(3) 0.0302(7) Uani 1 1 d .
H11 H 0.3857 0.6341 0.0599 0.036 Uiso 1 1 calc R
H12 H 0.2452 0.5841 0.1793 0.036 Uiso 1 1 calc R
C5 C 0.1812(3) 0.7442(3) 0.0172(3) 0.0274(7) Uani 1 1 d .
H13 H 0.2010 0.8219 0.0630 0.033 Uiso 1 1 calc R
H14 H 0.2126 0.7741 -0.0850 0.033 Uiso 1 1 calc R
C6 C -0.0647(3) 0.7360(3) 0.1827(3) 0.0226(6) Uani 1 1 d .
H15 H -0.0118 0.6779 0.2589 0.027 Uiso 1 1 calc R
H16 H -0.1724 0.7055 0.1959 0.027 Uiso 1 1 calc R
C7 C -0.0628(3) 0.8918(3) 0.1951(3) 0.0192(6) Uani 1 1 d .
H17 H 0.0433 0.9178 0.2012 0.023 Uiso 1 1 calc R
H18 H -0.0981 0.9523 0.1101 0.023 Uiso 1 1 calc R
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
O10 Co1 O8 173.35(8) 2_655 .
O10 Co1 OW1 97.68(8) 2_655 .
O8 Co1 OW1 88.66(7) . .
O10 Co1 O6 94.21(7) 2_655 .
O8 Co1 O6 79.24(7) . .
OW1 Co1 O6 165.73(7) . .
O10 Co1 O1 84.40(7) 2_655 .
O8 Co1 O1 96.96(7) . .
OW1 Co1 O1 95.85(8) . .
O6 Co1 O1 93.12(8) . .
O10 Co1 O9 78.90(7) 2_655 .
O8 Co1 O9 99.98(7) . .
OW1 Co1 O9 83.49(7) . .
O6 Co1 O9 91.13(7) . .
O1 Co1 O9 163.02(7) . .
O5 Co2 O5 180.0 . 2_666
O5 Co2 OW2 89.04(8) . 2_666
O5 Co2 OW2 90.96(8) 2_666 2_666
O5 Co2 OW2 90.96(8) . .
O5 Co2 OW2 89.04(8) 2_666 .
OW2 Co2 OW2 180.000(1) 2_666 .
O5 Co2 O7 80.14(7) . .
O5 Co2 O7 99.86(7) 2_666 .
OW2 Co2 O7 91.00(7) 2_666 .
OW2 Co2 O7 89.00(7) . .
O5 Co2 O7 99.86(7) . 2_666
O5 Co2 O7 80.14(7) 2_666 2_666
OW2 Co2 O7 89.00(7) 2_666 2_666
OW2 Co2 O7 91.00(7) . 2_666
O7 Co2 O7 180.0 . 2_666
N1 Co3 N1 180.00(13) 2_565 .
N1 Co3 N2 83.56(8) 2_565 2_565
N1 Co3 N2 96.44(8) . 2_565
N1 Co3 N2 96.44(8) 2_565 .
N1 Co3 N2 83.56(8) . .
N2 Co3 N2 180.00(10) 2_565 .
N1 Co3 O2 90.50(8) 2_565 2_565
N1 Co3 O2 89.50(8) . 2_565
N2 Co3 O2 92.79(8) 2_565 2_565
N2 Co3 O2 87.21(8) . 2_565
N1 Co3 O2 89.50(8) 2_565 .
N1 Co3 O2 90.50(8) . .
N2 Co3 O2 87.21(8) 2_565 .
N2 Co3 O2 92.79(8) . .
O2 Co3 O2 180.0 2_565 .
O2 S1 O3 109.55(14) . .
O2 S1 O4 109.91(12) . .
O3 S1 O4 109.59(12) . .
O2 S1 O1 109.14(11) . .
O3 S1 O1 107.85(13) . .
O4 S1 O1 110.77(11) . .
S1 O1 Co1 139.35(12) . .
S1 O2 Co3 138.04(11) . .
C1 O5 Co2 111.68(16) . .
C1 O6 Co1 112.69(17) . .
C2 O7 Co2 111.21(17) . .
C2 O8 Co1 113.54(17) . .
C3 O9 Co1 112.57(16) . .
C3 O10 Co1 115.12(16) . 2_655
Co1 OW1 H1 118.2 . .
Co1 OW1 H2 108.2 . .
H1 OW1 H2 105.6 . .
Co2 OW2 H3 116.0 . .
Co2 OW2 H4 120.4 . .
H3 OW2 H4 106.1 . .
C6 N2 C5 113.6(2) . .
C6 N2 Co3 117.64(16) . .
C5 N2 Co3 104.47(16) . .
C6 N2 H5 106.8 . .
C5 N2 H5 106.8 . .
Co3 N2 H5 106.8 . .
C7 N3 H6 109.5 . .
C7 N3 H7 109.5 . .
H6 N3 H7 109.5 . .
C7 N3 H8 109.5 . .
H6 N3 H8 109.5 . .
H7 N3 H8 109.5 . .
C4 N1 Co3 106.57(16) . .
C4 N1 H9 110.4 . .
Co3 N1 H9 110.4 . .
C4 N1 H10 110.4 . .
Co3 N1 H10 110.4 . .
H9 N1 H10 108.6 . .
O5 C1 O6 126.1(3) . .
O5 C1 C2 117.5(2) . .
O6 C1 C2 116.3(2) . .
O8 C2 O7 125.9(2) . .
O8 C2 C1 117.2(2) . .
O7 C2 C1 117.0(2) . .
O9 C3 O10 126.6(2) . .
O9 C3 C3 117.1(3) . 2_655
O10 C3 C3 116.3(3) . 2_655
N1 C4 C5 108.2(2) . .
N1 C4 H11 110.1 . .
C5 C4 H11 110.1 . .
N1 C4 H12 110.1 . .
C5 C4 H12 110.1 . .
H11 C4 H12 108.4 . .
N2 C5 C4 109.7(2) . .
N2 C5 H13 109.7 . .
C4 C5 H13 109.7 . .
N2 C5 H14 109.7 . .
C4 C5 H14 109.7 . .
H13 C5 H14 108.2 . .
N2 C6 C7 112.8(2) . .
N2 C6 H15 109.0 . .
C7 C6 H15 109.0 . .
N2 C6 H16 109.0 . .
C7 C6 H16 109.0 . .
H15 C6 H16 107.8 . .
N3 C7 C6 110.5(2) . .
N3 C7 H17 109.5 . .
C6 C7 H17 109.5 . .
N3 C7 H18 109.5 . .
C6 C7 H18 109.5 . .
H17 C7 H18 108.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O10 2.0676(18) 2_655
Co1 O8 2.0760(18) .
Co1 OW1 2.0964(19) .
Co1 O6 2.0977(19) .
Co1 O1 2.1108(17) .
Co1 O9 2.1419(17) .
Co2 O5 2.0871(18) .
Co2 O5 2.0871(18) 2_666
Co2 OW2 2.0911(18) 2_666
Co2 OW2 2.0911(18) .
Co2 O7 2.0971(18) .
Co2 O7 2.0971(18) 2_666
Co3 N1 2.093(2) 2_565
Co3 N1 2.093(2) .
Co3 N2 2.159(2) 2_565
Co3 N2 2.159(2) .
Co3 O2 2.2685(19) 2_565
Co3 O2 2.2685(19) .
S1 O2 1.462(2) .
S1 O3 1.463(2) .
S1 O4 1.468(2) .
S1 O1 1.4712(17) .
O5 C1 1.253(3) .
O6 C1 1.255(3) .
O7 C2 1.267(3) .
O8 C2 1.239(3) .
O9 C3 1.247(3) .
O10 C3 1.256(3) .
O10 Co1 2.0676(18) 2_655
OW1 H1 0.8461 .
OW1 H2 0.8475 .
OW2 H3 0.8419 .
OW2 H4 0.8454 .
N2 C6 1.472(3) .
N2 C5 1.485(3) .
N2 H5 0.9100 .
N3 C7 1.481(3) .
N3 H6 0.8900 .
N3 H7 0.8900 .
N3 H8 0.8900 .
N1 C4 1.476(4) .
N1 H9 0.9000 .
N1 H10 0.9000 .
C1 C2 1.539(4) .
C3 C3 1.551(5) 2_655
C4 C5 1.504(4) .
C4 H11 0.9700 .
C4 H12 0.9700 .
C5 H13 0.9700 .
C5 H14 0.9700 .
C6 C7 1.519(4) .
C6 H15 0.9700 .
C6 H16 0.9700 .
C7 H17 0.9700 .
C7 H18 0.9700 .
