#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:55:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179269 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/89/4318958.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_4318958
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 H32 Mn N4 O12 S2'
_chemical_formula_weight         663.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 95.186(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0833(14)
_cell_length_b                   8.2887(4)
_cell_length_c                   23.2228(15)
_cell_measurement_reflns_used    18962
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      1.68
_cell_volume                     2891.5(4)
_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 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            11593
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.36
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_T_max  1.1648
_exptl_absorpt_correction_T_min  0.7534
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.493
_exptl_crystal_size_mid          0.311
_exptl_crystal_size_min          0.299
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1200P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1689
_refine_ls_wR_factor_ref         0.1826
_reflns_number_gt                4298
_reflns_number_total             6413
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025915osi20021007_030312.cif
_cod_data_source_block           m068
_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               4318958
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Mn Mn 0.27146(4) 0.20550(6) 0.987717(19) 0.02971(17) Uani 1 1 d . . .
S1 S 0.14617(7) -0.26034(11) 0.88366(4) 0.0408(3) Uani 1 1 d . . .
S2 S 0.40480(7) -0.16592(11) 0.58950(4) 0.0377(2) Uani 1 1 d . . .
O1 O 0.1303(2) -0.4283(4) 0.89564(13) 0.0615(9) Uani 1 1 d . . .
O2 O 0.2401(2) -0.2221(4) 0.89143(13) 0.0555(8) Uani 1 1 d . . .
O3 O 0.0931(2) -0.1554(4) 0.91708(13) 0.0557(8) Uani 1 1 d . . .
O4 O 0.3100(2) -0.1514(4) 0.57013(13) 0.0578(8) Uani 1 1 d . . .
O5 O 0.4534(2) -0.0166(3) 0.58288(11) 0.0512(8) Uani 1 1 d . . .
O6 O 0.4461(2) -0.3008(4) 0.56222(12) 0.0508(7) Uani 1 1 d . . .
OW1 O 0.2226(2) 0.4484(3) 0.99286(11) 0.0486(7) Uani 1 1 d . . .
OW2 O 0.13299(19) 0.1171(3) 0.98075(11) 0.0455(7) Uani 1 1 d . . .
OW3 O 0.3178(2) -0.0397(3) 0.97976(12) 0.0516(8) Uani 1 1 d . . .
OW4 O 0.4102(2) 0.2768(4) 1.00318(12) 0.0466(7) Uani 1 1 d . . .
OW5 O -0.0028(3) 0.3244(5) 0.99986(16) 0.0716(10) Uani 1 1 d . . .
OW6 O 0.1523(4) -0.3315(8) 0.5679(2) 0.1254(19) Uani 1 1 d . . .
N1 N 0.2628(2) 0.2437(3) 0.89011(11) 0.0325(7) Uani 1 1 d . . .
N2 N 0.2653(2) 0.3020(4) 0.58570(11) 0.0352(7) Uani 1 1 d . . .
N3 N 0.0260(4) -0.1543(8) 0.63799(18) 0.0945(18) Uani 1 1 d . . .
H3A H -0.0204 -0.0966 0.6285 0.095 Uiso 1 1 calc R . .
H3B H 0.0547 -0.1975 0.6116 0.095 Uiso 1 1 calc R . .
N4 N 0.4325(3) -0.2644(5) 0.84323(14) 0.0563(10) Uani 1 1 d . . .
H4A H 0.4739 -0.3240 0.8599 0.056 Uiso 1 1 calc R . .
H4B H 0.3957 -0.2159 0.8635 0.056 Uiso 1 1 calc R . .
C1 C 0.2583(2) 0.2814(4) 0.76944(13) 0.0281(7) Uani 1 1 d . . .
C2 C 0.3187(3) 0.3644(5) 0.80710(13) 0.0354(8) Uani 1 1 d . . .
H2 H 0.3592 0.4351 0.7927 0.035 Uiso 1 1 calc R . .
C3 C 0.3185(3) 0.3416(5) 0.86613(14) 0.0387(9) Uani 1 1 d . . .
H3 H 0.3598 0.3983 0.8904 0.039 Uiso 1 1 calc R . .
C4 C 0.2029(3) 0.1687(5) 0.85381(14) 0.0424(9) Uani 1 1 d . . .
H4 H 0.1615 0.1025 0.8695 0.042 Uiso 1 1 calc R . .
C5 C 0.1985(3) 0.1834(5) 0.79459(14) 0.0420(9) Uani 1 1 d . . .
H5 H 0.1553 0.1273 0.7715 0.042 Uiso 1 1 calc R . .
C6 C 0.2590(2) 0.2946(4) 0.70553(13) 0.0284(7) Uani 1 1 d . . .
C7 C 0.1915(3) 0.2287(5) 0.66841(14) 0.0412(9) Uani 1 1 d . . .
H7 H 0.1427 0.1803 0.6831 0.041 Uiso 1 1 calc R . .
C8 C 0.1970(3) 0.2350(5) 0.61004(15) 0.0445(10) Uani 1 1 d . . .
H8 H 0.1508 0.1904 0.5859 0.044 Uiso 1 1 calc R . .
C9 C 0.3294(3) 0.3662(5) 0.62173(14) 0.0408(9) Uani 1 1 d . . .
H9 H 0.3775 0.4143 0.6061 0.041 Uiso 1 1 calc R . .
C10 C 0.3283(3) 0.3653(5) 0.68079(14) 0.0417(9) Uani 1 1 d . . .
H10 H 0.3747 0.4126 0.7040 0.042 Uiso 1 1 calc R . .
C11 C 0.1102(3) -0.2262(4) 0.81055(16) 0.0375(8) Uani 1 1 d . . .
C12 C 0.0352(3) -0.1328(5) 0.79493(17) 0.0446(9) Uani 1 1 d . . .
H12 H 0.0035 -0.0868 0.8233 0.045 Uiso 1 1 calc R . .
C13 C 0.0082(3) -0.1087(5) 0.73764(19) 0.0518(11) Uani 1 1 d . . .
H13 H -0.0416 -0.0452 0.7274 0.052 Uiso 1 1 calc R . .
C14 C 0.0538(3) -0.1774(6) 0.69473(19) 0.0532(11) Uani 1 1 d . . .
C15 C 0.1288(3) -0.2721(6) 0.71063(18) 0.0513(11) Uani 1 1 d . . .
H15 H 0.1601 -0.3195 0.6824 0.051 Uiso 1 1 calc R . .
C16 C 0.1560(3) -0.2949(5) 0.76806(18) 0.0449(9) Uani 1 1 d . . .
H16 H 0.2061 -0.3576 0.7784 0.045 Uiso 1 1 calc R . .
C17 C 0.4105(2) -0.2052(4) 0.66450(14) 0.0323(7) Uani 1 1 d . . .
C18 C 0.4760(3) -0.3027(5) 0.69122(15) 0.0362(8) Uani 1 1 d . . .
H18 H 0.5155 -0.3551 0.6690 0.036 Uiso 1 1 calc R . .
C19 C 0.4838(3) -0.3236(5) 0.75010(17) 0.0411(9) Uani 1 1 d . . .
H19 H 0.5284 -0.3895 0.7674 0.041 Uiso 1 1 calc R . .
C20 C 0.4252(3) -0.2466(4) 0.78398(16) 0.0376(8) Uani 1 1 d . . .
C21 C 0.3585(3) -0.1510(5) 0.75622(16) 0.0429(9) Uani 1 1 d . . .
H21 H 0.3179 -0.0999 0.7780 0.043 Uiso 1 1 calc R . .
C22 C 0.3515(3) -0.1307(5) 0.69766(16) 0.0409(9) Uani 1 1 d . . .
H22 H 0.3065 -0.0661 0.6801 0.041 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'
Mn Mn 0.3368 0.7283 '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
OW1 Mn OW3 178.03(10) . . ?
OW1 Mn OW4 93.79(12) . . ?
OW3 Mn OW4 87.47(12) . . ?
OW1 Mn OW2 89.32(12) . . ?
OW3 Mn OW2 89.58(12) . . ?
OW4 Mn OW2 173.70(11) . . ?
OW1 Mn N1 86.34(10) . . ?
OW3 Mn N1 92.03(11) . . ?
OW4 Mn N1 95.41(11) . . ?
OW2 Mn N1 90.24(11) . . ?
OW1 Mn N2 85.71(11) . 4_566 ?
OW3 Mn N2 95.86(11) . 4_566 ?
OW4 Mn N2 88.19(11) . 4_566 ?
OW2 Mn N2 86.58(11) . 4_566 ?
N1 Mn N2 171.47(11) . 4_566 ?
O2 S1 O1 111.4(2) . . ?
O2 S1 O3 112.48(19) . . ?
O1 S1 O3 111.4(2) . . ?
O2 S1 C11 107.36(19) . . ?
O1 S1 C11 107.42(17) . . ?
O3 S1 C11 106.41(19) . . ?
O5 S2 O6 111.69(18) . . ?
O5 S2 O4 112.62(19) . . ?
O6 S2 O4 112.0(2) . . ?
O5 S2 C17 106.33(16) . . ?
O6 S2 C17 107.69(17) . . ?
O4 S2 C17 106.08(18) . . ?
C3 N1 C4 116.0(3) . . ?
C3 N1 Mn 121.4(2) . . ?
C4 N1 Mn 122.6(2) . . ?
C9 N2 C8 116.3(3) . . ?
C9 N2 Mn 122.9(2) . 4_565 ?
C8 N2 Mn 120.7(2) . 4_565 ?
C14 N3 H3A 120.0 . . ?
C14 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C20 N4 H4A 120.0 . . ?
C20 N4 H4B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
C5 C1 C2 116.2(3) . . ?
C5 C1 C6 121.9(3) . . ?
C2 C1 C6 121.9(3) . . ?
C1 C2 C3 119.7(3) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
N1 C3 C2 123.9(3) . . ?
N1 C3 H3 118.0 . . ?
C2 C3 H3 118.0 . . ?
N1 C4 C5 124.0(4) . . ?
N1 C4 H4 118.0 . . ?
C5 C4 H4 118.0 . . ?
C1 C5 C4 120.0(3) . . ?
C1 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C10 C6 C7 117.0(3) . . ?
C10 C6 C1 121.6(3) . . ?
C7 C6 C1 121.3(3) . . ?
C8 C7 C6 119.6(4) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
N2 C8 C7 123.6(4) . . ?
N2 C8 H8 118.2 . . ?
C7 C8 H8 118.2 . . ?
N2 C9 C10 123.5(3) . . ?
N2 C9 H9 118.3 . . ?
C10 C9 H9 118.3 . . ?
C6 C10 C9 120.0(3) . . ?
C6 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C16 C11 C12 119.5(4) . . ?
C16 C11 S1 119.6(3) . . ?
C12 C11 S1 120.9(3) . . ?
C13 C12 C11 119.8(4) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C14 C13 C12 121.1(4) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C13 C14 N3 120.7(4) . . ?
C13 C14 C15 118.9(4) . . ?
N3 C14 C15 120.4(5) . . ?
C16 C15 C14 119.9(4) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C11 C16 C15 120.9(4) . . ?
C11 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C22 C17 C18 119.0(3) . . ?
C22 C17 S2 119.6(3) . . ?
C18 C17 S2 121.3(3) . . ?
C17 C18 C19 121.0(4) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 H18 119.5 . . ?
C20 C19 C18 120.3(4) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
N4 C20 C19 121.2(4) . . ?
N4 C20 C21 120.8(4) . . ?
C19 C20 C21 118.0(3) . . ?
C22 C21 C20 121.2(4) . . ?
C22 C21 H21 119.4 . . ?
C20 C21 H21 119.4 . . ?
C21 C22 C17 120.5(4) . . ?
C21 C22 H22 119.8 . . ?
C17 C22 H22 119.8 . . ?
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
Mn OW1 2.151(3) . ?
Mn OW3 2.163(3) . ?
Mn OW4 2.173(3) . ?
Mn OW2 2.206(3) . ?
Mn N1 2.281(3) . ?
Mn N2 2.287(3) 4_566 ?
S1 O2 1.447(3) . ?
S1 O1 1.444(3) . ?
S1 O3 1.453(3) . ?
S1 C11 1.758(4) . ?
S2 O5 1.453(3) . ?
S2 O6 1.453(3) . ?
S2 O4 1.464(3) . ?
S2 C17 1.766(3) . ?
N1 C3 1.326(5) . ?
N1 C4 1.332(5) . ?
N2 C9 1.332(5) . ?
N2 C8 1.339(5) . ?
N2 Mn 2.287(3) 4_565 ?
N3 C14 1.360(6) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
N4 C20 1.378(5) . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
C1 C5 1.382(5) . ?
C1 C2 1.387(5) . ?
C1 C6 1.489(4) . ?
C2 C3 1.384(4) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.376(4) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C10 1.369(5) . ?
C6 C7 1.386(5) . ?
C7 C8 1.367(5) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C10 1.373(5) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C16 1.378(6) . ?
C11 C12 1.392(6) . ?
C12 C13 1.370(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.383(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.399(6) . ?
C15 C16 1.373(6) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C22 1.374(5) . ?
C17 C18 1.380(5) . ?
C18 C19 1.373(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.391(6) . ?
C19 H19 0.9300 . ?
C20 C21 1.393(6) . ?
C21 C22 1.365(5) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
