#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:32:08 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179065 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/27/4302760.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_4302760
loop_
_publ_author_name
'Tori Z. Forbes'
'Slavi C. Sevov'
_publ_contact_author_address
;Department of Chemistry
University of Notre Dame
Notre Dame, IN 46556
;
_publ_contact_author_email       ssevov@nd.edu
_publ_contact_author_name        'Slavi C. Sevov'
_publ_section_title
;
Metal-Organic Frameworks with Direct Transition Metal-Sulfonate
Interactions and Charge-Assisted Hydrogen Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6873
_journal_page_last               6878
_journal_paper_doi               10.1021/ic9007922
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C22 H22 Co N8 O6 S2'
_chemical_formula_weight         617.55
_chemical_name_common            (Co(Im)4)15NDS
_chemical_name_systematic
; 
 cobalt tetraimidazole 1,5-napthalene disulfonate
;
_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                60.601(2)
_cell_angle_beta                 86.866(2)
_cell_angle_gamma                73.920(2)
_cell_formula_units_Z            1
_cell_length_a                   8.2318(4)
_cell_length_b                   9.7087(5)
_cell_length_c                   9.7569(5)
_cell_measurement_reflns_used    363
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      58
_cell_measurement_theta_min      2.5
_cell_volume                     649.69(6)
_computing_cell_refinement       'APEX II (Bruker, 2005)'
_computing_data_collection       'APEX II (Bruker, 2005)'
_computing_data_reduction        'APEX II (Bruker, 2005)'
_computing_molecular_graphics    'Crystalmaker version 1.3.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 'not measured'
_diffrn_measured_fraction_theta_full 0.897
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_device_type  'Bruker APEX II diffractometer'
_diffrn_measurement_method       ω
_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  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38533
_diffrn_reflns_theta_full        43.36
_diffrn_reflns_theta_max         43.36
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  0.7622
_exptl_absorpt_correction_T_min  0.5783
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocky
_exptl_crystal_F_000             317
_exptl_crystal_size_max          0.680
_exptl_crystal_size_mid          0.530
_exptl_crystal_size_min          0.320
_refine_diff_density_max         1.664
_refine_diff_density_min         -1.410
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         8785
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0581P)²+0.1356P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                7321
_reflns_number_total             8785
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9007922_si_002_5.cif
_cod_data_source_block           compound4
_cod_database_code               4302760
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.5000 0.5000 0.5000 0.00921(4) Uani 1 2 d S . .
S1 S 0.25314(3) 0.92274(2) 0.31249(2) 0.00927(4) Uani 1 1 d . . .
O1 O 0.19740(10) 0.94875(8) 0.44412(7) 0.01485(11) Uani 1 1 d . . .
O2 O 0.33190(10) 0.74987(8) 0.36095(8) 0.01515(11) Uani 1 1 d . . .
O3 O 0.35986(10) 1.02608(9) 0.21723(8) 0.01630(12) Uani 1 1 d . . .
N1 N 0.38001(11) 0.46748(9) 0.70645(8) 0.01322(12) Uani 1 1 d . . .
N4 N 0.30840(13) 0.33257(11) 0.94700(10) 0.02028(16) Uani 1 1 d D . .
N3 N 0.19667(12) 0.25589(11) 0.40781(11) 0.01884(15) Uani 1 1 d D . .
N2 N 0.32198(11) 0.41345(9) 0.43801(9) 0.01350(12) Uani 1 1 d . . .
C1 C -0.08650(12) 1.03903(11) 0.23516(9) 0.01367(13) Uani 1 1 d D . .
C2 C -0.23439(12) 1.07775(12) 0.00634(10) 0.01470(14) Uani 1 1 d D . .
C3 C 0.35548(13) 0.32676(11) 0.81544(11) 0.01683(15) Uani 1 1 d D . .
C4 C -0.23842(13) 1.08509(13) 0.14304(11) 0.01696(15) Uani 1 1 d D . .
C5 C 0.34518(15) 0.56922(12) 0.77170(11) 0.01841(16) Uani 1 1 d D . .
C6 C 0.30204(16) 0.48637(14) 0.92166(12) 0.02238(19) Uani 1 1 d D . .
C7 C 0.33506(16) 0.26422(13) 0.46440(17) 0.0268(2) Uani 1 1 d D . .
C8 C 0.0902(2) 0.4104(2) 0.3337(3) 0.0664(8) Uani 1 1 d D . .
C9 C 0.1688(2) 0.50616(18) 0.3538(3) 0.0631(7) Uani 1 1 d D . .
C10 C 0.07731(11) 0.97593(9) 0.04609(8) 0.00991(11) Uani 1 1 d . . .
C11 C 0.06696(11) 0.98468(9) 0.18845(8) 0.01003(11) Uani 1 1 d . . .
H10 H 0.135(3) 0.625(3) 0.307(3) 0.050 Uiso 1 1 d D . .
H9 H -0.026(3) 0.443(3) 0.280(3) 0.050 Uiso 1 1 d D . .
H3 H 0.364(3) 0.230(3) 0.806(3) 0.050 Uiso 1 1 d D . .
H4 H -0.093(3) 1.042(3) 0.329(3) 0.050 Uiso 1 1 d D . .
H5 H -0.338(3) 1.112(3) -0.055(3) 0.050 Uiso 1 1 d D . .
H6 H 0.353(3) 0.678(3) 0.712(3) 0.050 Uiso 1 1 d D . .
H8 H -0.349(3) 1.120(3) 0.174(3) 0.050 Uiso 1 1 d D . .
H1 H 0.180(3) 0.164(3) 0.422(3) 0.050 Uiso 1 1 d D . .
H2 H 0.310(3) 0.246(3) 1.039(3) 0.050 Uiso 1 1 d D . .
H11 H 0.270(3) 0.510(3) 1.006(3) 0.050 Uiso 1 1 d D . .
H13 H 0.430(3) 0.164(3) 0.516(3) 0.050 Uiso 1 1 d D . .
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'
Co Co 0.3494 0.9721 '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'
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
N1 Co1 N1 180.0 . 2_666 ?
N1 Co1 N2 90.17(3) . . ?
N1 Co1 N2 89.83(3) 2_666 . ?
N1 Co1 N2 89.83(3) . 2_666 ?
N1 Co1 N2 90.17(3) 2_666 2_666 ?
N2 Co1 N2 180.0 . 2_666 ?
N1 Co1 O2 88.20(3) . 2_666 ?
N1 Co1 O2 91.80(3) 2_666 2_666 ?
N2 Co1 O2 91.75(3) . 2_666 ?
N2 Co1 O2 88.25(3) 2_666 2_666 ?
N1 Co1 O2 91.80(3) . . ?
N1 Co1 O2 88.20(3) 2_666 . ?
N2 Co1 O2 88.25(3) . . ?
N2 Co1 O2 91.75(3) 2_666 . ?
O2 Co1 O2 180.000(1) 2_666 . ?
O2 S1 O1 112.87(4) . . ?
O2 S1 O3 111.99(5) . . ?
O1 S1 O3 112.39(4) . . ?
O2 S1 C11 105.75(4) . . ?
O1 S1 C11 106.45(4) . . ?
O3 S1 C11 106.80(4) . . ?
S1 O2 Co1 157.80(4) . . ?
C3 N1 C5 105.82(7) . . ?
C3 N1 Co1 124.25(6) . . ?
C5 N1 Co1 128.65(6) . . ?
C3 N4 C6 107.71(8) . . ?
C3 N4 H2 124.1(15) . . ?
C6 N4 H2 126.2(15) . . ?
C7 N3 C8 106.71(9) . . ?
C7 N3 H1 124.5(16) . . ?
C8 N3 H1 128.8(16) . . ?
C7 N2 C9 104.41(9) . . ?
C7 N2 Co1 129.34(7) . . ?
C9 N2 Co1 126.20(7) . . ?
C11 C1 C4 119.87(7) . . ?
C11 C1 H4 121.4(15) . . ?
C4 C1 H4 118.7(15) . . ?
C4 C2 C10 120.79(9) . 2_575 ?
C4 C2 H5 119.1(14) . . ?
C10 C2 H5 120.1(14) 2_575 . ?
N1 C3 N4 111.21(8) . . ?
N1 C3 H3 127.3(14) . . ?
N4 C3 H3 121.5(14) . . ?
C2 C4 C1 120.60(8) . . ?
C2 C4 H8 117.3(13) . . ?
C1 C4 H8 122.1(13) . . ?
C6 C5 N1 109.51(9) . . ?
C6 C5 H6 130.7(14) . . ?
N1 C5 H6 119.8(14) . . ?
C5 C6 N4 105.75(9) . . ?
C5 C6 H11 136.4(14) . . ?
N4 C6 H11 117.8(14) . . ?
N2 C7 N3 112.52(10) . . ?
N2 C7 H13 129.2(14) . . ?
N3 C7 H13 118.2(14) . . ?
N3 C8 C9 106.13(12) . . ?
N3 C8 H9 125.4(14) . . ?
C9 C8 H9 128.4(13) . . ?
N2 C9 C8 110.16(12) . . ?
N2 C9 H10 120.5(15) . . ?
C8 C9 H10 128.9(15) . . ?
C2 C10 C10 119.36(8) 2_575 2_575 ?
C2 C10 C11 122.72(8) 2_575 . ?
C10 C10 C11 117.92(9) 2_575 . ?
C1 C11 C10 121.45(8) . . ?
C1 C11 S1 117.71(6) . . ?
C10 C11 S1 120.84(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
Co1 N1 2.1127(7) . ?
Co1 N1 2.1127(7) 2_666 ?
Co1 N2 2.1207(7) . ?
Co1 N2 2.1207(7) 2_666 ?
Co1 O2 2.1806(7) 2_666 ?
Co1 O2 2.1806(6) . ?
S1 O2 1.4534(7) . ?
S1 O1 1.4537(6) . ?
S1 O3 1.4579(7) . ?
S1 C11 1.7757(9) . ?
N1 C3 1.3196(11) . ?
N1 C5 1.3797(12) . ?
N4 C3 1.3437(13) . ?
N4 C6 1.3745(15) . ?
N4 H2 0.88(2) . ?
N3 C7 1.3315(14) . ?
N3 C8 1.3480(19) . ?
N3 H1 0.88(2) . ?
N2 C7 1.3142(12) . ?
N2 C9 1.3544(17) . ?
C1 C11 1.3733(12) . ?
C1 C4 1.4107(14) . ?
C1 H4 0.93(2) . ?
C2 C4 1.3683(12) . ?
C2 C10 1.4218(12) 2_575 ?
C2 H5 0.95(2) . ?
C3 H3 0.97(2) . ?
C4 H8 0.96(2) . ?
C5 C6 1.3638(13) . ?
C5 H6 0.94(2) . ?
C6 H11 0.96(2) . ?
C7 H13 0.98(3) . ?
C8 C9 1.3588(19) . ?
C8 H9 1.00(2) . ?
C9 H10 0.97(2) . ?
C10 C2 1.4218(12) 2_575 ?
C10 C10 1.4249(16) 2_575 ?
C10 C11 1.4292(10) . ?
