#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:55:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179269 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/89/4318957.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_4318957
loop_
_publ_author_name
'Yonghui Wang'
'Liyun Feng'
'Yangguang Li'
'Changwen Hu'
'Enbo Wang'
'Ninghai Hu'
'Hengqing Jia'
_publ_section_title
;
 Novel Hydrogen-Bonded Three-Dimensional Networks Encapsulating
 One-Dimensional Covalent Chains: [M(4,4'-bipy)(H2O)4](4-abs)2.nH2O
 (4,4'-bipy = 4,4'-Bipyridine; 4-abs = 4-Aminobenzenesulfonate) (M = Co, n
 = 1; M = Mn, n = 2)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6351
_journal_page_last               6357
_journal_paper_doi               10.1021/ic025915o
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C22 H30 Co N4 O11 S2'
_chemical_formula_weight         649.55
_chemical_name_systematic
; 
 ? 
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.82(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.380(2)
_cell_length_b                   8.0274(16)
_cell_length_c                   15.670(3)
_cell_measurement_reflns_used    5798
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.35
_cell_measurement_theta_min      2.27
_cell_volume                     1429.7(5)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '100x100 microns'
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Rigaku RAPID'
_diffrn_measurement_method       Oscillation
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0746
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5798
_diffrn_reflns_theta_full        27.35
_diffrn_reflns_theta_max         27.35
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.702
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             674
_exptl_crystal_size_max          0.424
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.181
_refine_diff_density_max         2.127
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.22(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5798
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0814
_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)+(0.1373P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1977
_refine_ls_wR_factor_ref         0.2078
_reflns_number_gt                4154
_reflns_number_total             5798
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025915osi20021007_030311.cif
_cod_data_source_block           m093
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4318957
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -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_assembly
_atom_site_disorder_group
Co Co 0.01334(6) 0.80486(12) 0.22655(5) 0.0394(2) Uani 1 1 d . . .
S1 S 0.79055(16) 0.8434(2) 0.63246(12) 0.0549(5) Uani 1 1 d . . .
S2 S 0.19125(15) 0.7613(2) 0.91390(12) 0.0483(4) Uani 1 1 d . . .
OW1 O 0.0243(4) 0.5506(6) 0.1914(4) 0.0618(14) Uani 1 1 d . . .
OW2 O -0.0053(4) 0.8698(7) 0.0985(3) 0.0568(14) Uani 1 1 d . . .
OW3 O 0.0217(5) 0.7288(7) 0.3546(3) 0.0560(13) Uani 1 1 d . . .
OW4 O 0.0024(4) 1.0573(7) 0.2631(4) 0.0586(13) Uani 1 1 d . . .
OW5 O 0.0122(14) 0.9548(14) 0.4764(7) 0.089(5) Uani 0.50 1 d P . .
OW6 O 0.1589(13) 0.929(2) 0.6643(9) 0.096(5) Uani 0.50 1 d P . .
O1 O 0.8170(6) 1.0006(8) 0.5924(4) 0.0752(18) Uani 1 1 d . . .
O2 O 0.8080(6) 0.8473(11) 0.7241(4) 0.089(2) Uani 1 1 d . . .
O3 O 0.8592(6) 0.7093(10) 0.5979(5) 0.093(2) Uani 1 1 d . . .
O4 O 0.1394(5) 0.8962(8) 0.9588(5) 0.083(2) Uani 1 1 d . . .
O5 O 0.1751(5) 0.5976(7) 0.9522(4) 0.0661(16) Uani 1 1 d . . .
O6 O 0.1482(5) 0.7645(9) 0.8245(4) 0.078(2) Uani 1 1 d . . .
N1 N -0.1756(4) 0.7991(9) 0.2294(3) 0.0417(11) Uani 1 1 d . . .
N2 N -0.7989(4) 0.8026(9) 0.2319(3) 0.0419(11) Uani 1 1 d . . .
N3 N 0.2885(6) 0.7321(12) 0.5484(6) 0.086(2) Uani 1 1 d . . .
H3A H 0.2639 0.6728 0.5054 0.086 Uiso 1 1 calc R . .
H3B H 0.2388 0.7786 0.5805 0.086 Uiso 1 1 calc R . .
N4 N 0.7091(5) 0.8244(12) 0.9268(4) 0.0692(18) Uani 1 1 d . . .
H4A H 0.7455 0.8792 0.9671 0.069 Uiso 1 1 calc R . .
H4B H 0.7484 0.7725 0.8895 0.069 Uiso 1 1 calc R . .
C1 C -0.2312(6) 0.8687(10) 0.2944(4) 0.0497(18) Uani 1 1 d . . .
H1 H -0.1857 0.9214 0.3373 0.050 Uiso 1 1 calc R . .
C2 C -0.3523(5) 0.8663(9) 0.3010(4) 0.0473(16) Uani 1 1 d . . .
H2 H -0.3868 0.9158 0.3473 0.047 Uiso 1 1 calc R . .
C3 C -0.4209(5) 0.7882(9) 0.2371(3) 0.0341(12) Uani 1 1 d . . .
C4 C -0.3629(5) 0.7198(9) 0.1697(4) 0.0453(16) Uani 1 1 d . . .
H4 H -0.4055 0.6680 0.1250 0.045 Uiso 1 1 calc R . .
C5 C -0.2430(5) 0.7284(9) 0.1691(4) 0.0435(15) Uani 1 1 d . . .
H5 H -0.2066 0.6813 0.1230 0.044 Uiso 1 1 calc R . .
C6 C -0.5516(4) 0.7929(8) 0.2373(3) 0.0330(11) Uani 1 1 d . . .
C7 C -0.6110(6) 0.8704(10) 0.3013(4) 0.0483(17) Uani 1 1 d . . .
H7 H -0.5693 0.9206 0.3469 0.048 Uiso 1 1 calc R . .
C8 C -0.7327(5) 0.8729(9) 0.2970(4) 0.0453(16) Uani 1 1 d . . .
H8 H -0.7711 0.9251 0.3407 0.045 Uiso 1 1 calc R . .
C9 C -0.7405(5) 0.7343(10) 0.1706(4) 0.0457(15) Uani 1 1 d . . .
H9 H -0.7836 0.6914 0.1236 0.046 Uiso 1 1 calc R . .
C10 C -0.6203(5) 0.7220(9) 0.1713(4) 0.0412(14) Uani 1 1 d . . .
H10 H -0.5848 0.6660 0.1274 0.041 Uiso 1 1 calc R . .
C11 C 0.6413(5) 0.8027(10) 0.6091(4) 0.0429(13) Uani 1 1 d . . .
C12 C 0.6073(7) 0.7044(9) 0.5389(5) 0.0560(18) Uani 1 1 d . . .
H12 H 0.6637 0.6540 0.5065 0.056 Uiso 1 1 calc R . .
C13 C 0.4860(7) 0.6820(10) 0.5175(5) 0.062(2) Uani 1 1 d . . .
H13 H 0.4623 0.6187 0.4700 0.062 Uiso 1 1 calc R . .
C14 C 0.4054(7) 0.7521(10) 0.5657(5) 0.0553(18) Uani 1 1 d . . .
C15 C 0.4396(7) 0.8525(11) 0.6365(5) 0.060(2) Uani 1 1 d . . .
H15 H 0.3833 0.9038 0.6687 0.060 Uiso 1 1 calc R . .
C16 C 0.5603(7) 0.8738(9) 0.6578(4) 0.0523(17) Uani 1 1 d . . .
H16 H 0.5843 0.9367 0.7053 0.052 Uiso 1 1 calc R . .
C17 C 0.5893(5) 0.8196(11) 0.9219(4) 0.0485(15) Uani 1 1 d . . .
C18 C 0.5306(6) 0.7239(9) 0.8568(4) 0.0498(16) Uani 1 1 d . . .
H18 H 0.5733 0.6694 0.8161 0.050 Uiso 1 1 calc R . .
C19 C 0.4102(6) 0.7123(9) 0.8542(4) 0.0483(16) Uani 1 1 d . . .
H19 H 0.3718 0.6497 0.8114 0.048 Uiso 1 1 calc R . .
C20 C 0.3444(5) 0.7921(9) 0.9143(4) 0.0405(13) Uani 1 1 d . . .
C21 C 0.4032(6) 0.8877(8) 0.9772(4) 0.0418(14) Uani 1 1 d . . .
H21 H 0.3599 0.9427 1.0174 0.042 Uiso 1 1 calc R . .
C22 C 0.5234(6) 0.9023(9) 0.9812(4) 0.0482(17) Uani 1 1 d . . .
H22 H 0.5608 0.9674 1.0235 0.048 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
_geom_angle_publ_flag
OW2 Co OW3 176.0(2) . . ?
OW2 Co OW4 91.0(2) . . ?
OW3 Co OW4 91.2(2) . . ?
OW2 Co OW1 89.7(2) . . ?
OW3 Co OW1 88.2(2) . . ?
OW4 Co OW1 179.3(3) . . ?
OW2 Co N2 95.4(2) . 1_655 ?
OW3 Co N2 87.8(2) . 1_655 ?
OW4 Co N2 94.0(2) . 1_655 ?
OW1 Co N2 86.0(2) . 1_655 ?
OW2 Co N1 88.3(2) . . ?
OW3 Co N1 88.4(2) . . ?
OW4 Co N1 86.7(2) . . ?
OW1 Co N1 93.2(2) . . ?
N2 Co N1 176.2(2) 1_655 . ?
O2 S1 O1 113.1(5) . . ?
O2 S1 O3 109.7(5) . . ?
O1 S1 O3 111.0(4) . . ?
O2 S1 C11 107.3(3) . . ?
O1 S1 C11 107.0(4) . . ?
O3 S1 C11 108.6(4) . . ?
O4 S2 O6 109.3(4) . . ?
O4 S2 O5 114.5(4) . . ?
O6 S2 O5 111.5(4) . . ?
O4 S2 C20 108.9(4) . . ?
O6 S2 C20 106.7(3) . . ?
O5 S2 C20 105.6(4) . . ?
C5 N1 C1 116.3(5) . . ?
C5 N1 Co 122.8(4) . . ?
C1 N1 Co 120.9(4) . . ?
C9 N2 C8 116.0(5) . . ?
C9 N2 Co 121.1(4) . 1_455 ?
C8 N2 Co 122.9(4) . 1_455 ?
N1 C1 C2 123.8(6) . . ?
C1 C2 C3 118.5(6) . . ?
C4 C3 C2 117.2(5) . . ?
C4 C3 C6 121.7(5) . . ?
C2 C3 C6 120.9(5) . . ?
C5 C4 C3 119.9(6) . . ?
N1 C5 C4 124.2(6) . . ?
C7 C6 C10 116.5(5) . . ?
C7 C6 C3 122.4(5) . . ?
C10 C6 C3 121.0(5) . . ?
C6 C7 C8 119.6(6) . . ?
N2 C8 C7 123.2(5) . . ?
N2 C9 C10 124.3(6) . . ?
C9 C10 C6 120.1(6) . . ?
C16 C11 C12 121.0(6) . . ?
C16 C11 S1 119.0(5) . . ?
C12 C11 S1 120.0(5) . . ?
C11 C12 C13 119.2(7) . . ?
C14 C13 C12 120.0(7) . . ?
C13 C14 N3 122.1(7) . . ?
C13 C14 C15 120.9(7) . . ?
N3 C14 C15 117.1(8) . . ?
C16 C15 C14 118.9(7) . . ?
C11 C16 C15 120.0(7) . . ?
N4 C17 C22 121.3(7) . . ?
N4 C17 C18 119.4(7) . . ?
C22 C17 C18 119.3(6) . . ?
C19 C18 C17 119.5(6) . . ?
C18 C19 C20 121.3(6) . . ?
C19 C20 C21 118.6(6) . . ?
C19 C20 S2 120.0(5) . . ?
C21 C20 S2 121.3(5) . . ?
C22 C21 C20 121.4(6) . . ?
C21 C22 C17 119.9(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co OW2 2.073(5) . ?
Co OW3 2.095(5) . ?
Co OW4 2.111(6) . ?
Co OW1 2.119(5) . ?
Co N2 2.134(4) 1_655 ?
Co N1 2.154(4) . ?
S1 O2 1.440(6) . ?
S1 O1 1.448(6) . ?
S1 O3 1.451(7) . ?
S1 C11 1.751(6) . ?
S2 O4 1.434(6) . ?
S2 O6 1.461(6) . ?
S2 O5 1.461(6) . ?
S2 C20 1.761(6) . ?
N1 C5 1.316(8) . ?
N1 C1 1.346(8) . ?
N2 C9 1.315(8) . ?
N2 C8 1.360(8) . ?
N2 Co 2.134(4) 1_455 ?
N3 C14 1.354(10) . ?
N4 C17 1.363(8) . ?
C1 C2 1.388(8) . ?
C2 C3 1.389(9) . ?
C3 C4 1.386(8) . ?
C3 C6 1.488(7) . ?
C4 C5 1.367(8) . ?
C6 C7 1.384(9) . ?
C6 C10 1.388(8) . ?
C7 C8 1.384(8) . ?
C9 C10 1.371(8) . ?
C11 C16 1.352(10) . ?
C11 C12 1.392(10) . ?
C12 C13 1.416(11) . ?
C13 C14 1.341(11) . ?
C14 C15 1.411(11) . ?
C15 C16 1.407(11) . ?
C17 C22 1.391(10) . ?
C17 C18 1.418(10) . ?
C18 C19 1.372(10) . ?
C19 C20 1.388(9) . ?
C20 C21 1.394(9) . ?
C21 C22 1.372(10) . ?
