#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:38:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179120 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/82/4308269.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_4308269
loop_
_publ_author_name
'Xin-Yi Wang'
'Rachelle Justice'
'Slavi C. Sevov'
_publ_section_title
;
Hydrogen-Bonded Metal-Complex Sulfonate (MCS) Inclusion Compounds: Effect
of the Guest Molecule on the Host Framework
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4626
_journal_page_last               4631
_journal_paper_doi               10.1021/ic070324p
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety
'2(C12 H8 O6 S2), (C12 H8 O6 S2), 2(Co H18 N6), 2(C2 H3 N), 4(H2 O)'
_chemical_formula_sum            'C40 H74 Co2 N14 O22 S6'
_chemical_formula_weight         1413.36
_chemical_name_common            CoHA-BPDS-MeCN
_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                100.318(2)
_cell_angle_beta                 93.647(2)
_cell_angle_gamma                96.525(2)
_cell_formula_units_Z            1
_cell_length_a                   7.7896(3)
_cell_length_b                   13.1339(5)
_cell_length_c                   15.6698(5)
_cell_measurement_temperature    100(2)
_cell_volume                     1561.21(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL-V5.1'
_computing_molecular_graphics    Diomand
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21617
_diffrn_reflns_theta_full        26.77
_diffrn_reflns_theta_max         26.77
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_T_max  0.9760
_exptl_absorpt_correction_T_min  0.8946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Blessing, R.H. (1995) Acta Cryst. A51, 33-38'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             738
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.797
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         6596
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0715
_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)+(0.0203P)²+20.1701P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1862
_refine_ls_wR_factor_ref         0.1902
_reflns_number_gt                5440
_reflns_number_total             6596
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070324p-file001_5.cif
_cod_data_source_block           CoHA-BPDS-MeCN
_cod_database_code               4308269
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 0.0000 0.0000 1.0000 0.0094(2) Uani 1 2 d S . .
Co2 Co 0.5000 0.5000 1.0000 0.0122(2) Uani 1 2 d S . .
S1 S 0.08255(19) 0.24451(11) 0.82056(9) 0.0159(3) Uani 1 1 d . . .
S2 S 0.07257(18) 0.36399(11) 0.16696(9) 0.0143(3) Uani 1 1 d . . .
S3 S 0.52458(18) 0.05557(11) 0.17407(9) 0.0135(3) Uani 1 1 d . . .
N1 N 0.0374(6) 0.0301(4) 1.1281(3) 0.0128(9) Uani 1 1 d . . .
H1A H -0.0547 0.0587 1.1508 0.019 Uiso 1 1 calc R . .
H1B H 0.1357 0.0757 1.1449 0.019 Uiso 1 1 calc R . .
H1C H 0.0485 -0.0302 1.1477 0.019 Uiso 1 1 calc R . .
N2 N 0.1292(6) -0.1195(4) 0.9952(3) 0.0140(10) Uani 1 1 d . . .
H2A H 0.1913 -0.1149 1.0473 0.021 Uiso 1 1 calc R . .
H2B H 0.2027 -0.1198 0.9523 0.021 Uiso 1 1 calc R . .
H2C H 0.0538 -0.1794 0.9839 0.021 Uiso 1 1 calc R . .
N3 N 0.2147(6) 0.0883(4) 0.9923(3) 0.0136(9) Uani 1 1 d . . .
H3A H 0.3059 0.0513 0.9961 0.020 Uiso 1 1 calc R . .
H3B H 0.2282 0.1444 1.0368 0.020 Uiso 1 1 calc R . .
H3C H 0.2104 0.1106 0.9406 0.020 Uiso 1 1 calc R . .
N4 N 0.4220(6) 0.3551(4) 1.0061(3) 0.0163(10) Uani 1 1 d . . .
H4A H 0.4636 0.3120 0.9622 0.025 Uiso 1 1 calc R . .
H4B H 0.3041 0.3441 1.0007 0.025 Uiso 1 1 calc R . .
H4C H 0.4621 0.3416 1.0582 0.025 Uiso 1 1 calc R . .
N5 N 0.2608(6) 0.5331(4) 1.0103(3) 0.0185(11) Uani 1 1 d . . .
H5A H 0.1872 0.4863 0.9709 0.028 Uiso 1 1 calc R . .
H5B H 0.2541 0.5986 0.9999 0.028 Uiso 1 1 calc R . .
H5C H 0.2307 0.5298 1.0650 0.028 Uiso 1 1 calc R . .
N6 N 0.4548(7) 0.4631(4) 0.8734(3) 0.0174(10) Uani 1 1 d . . .
H6A H 0.5177 0.4112 0.8525 0.026 Uiso 1 1 calc R . .
H6B H 0.4859 0.5201 0.8496 0.026 Uiso 1 1 calc R . .
H6C H 0.3399 0.4409 0.8593 0.026 Uiso 1 1 calc R . .
O1 O -0.0807(5) 0.1818(3) 0.8282(3) 0.0202(9) Uani 1 1 d . . .
O2 O 0.0950(6) 0.3488(3) 0.8736(3) 0.0254(10) Uani 1 1 d . . .
O3 O 0.2304(6) 0.1897(4) 0.8363(3) 0.0259(10) Uani 1 1 d . . .
O4 O -0.1037(6) 0.3777(4) 0.1382(3) 0.0247(10) Uani 1 1 d . . .
O5 O 0.1338(6) 0.2752(3) 0.1134(3) 0.0216(9) Uani 1 1 d . . .
O6 O 0.1926(6) 0.4594(3) 0.1755(3) 0.0207(9) Uani 1 1 d . . .
O7 O 0.7023(5) 0.0966(4) 0.1637(3) 0.0195(9) Uani 1 1 d . . .
O8 O 0.4631(6) -0.0432(3) 0.1161(3) 0.0210(9) Uani 1 1 d . . .
O9 O 0.4043(5) 0.1331(3) 0.1680(3) 0.0161(8) Uani 1 1 d . . .
C1 C 0.0819(8) 0.2613(5) 0.7105(4) 0.0161(12) Uani 1 1 d . . .
C2 C 0.1505(9) 0.1909(5) 0.6497(4) 0.0251(14) Uani 1 1 d . . .
H2 H 0.2016 0.1347 0.6670 0.030 Uiso 1 1 calc R . .
C3 C 0.0059(8) 0.3431(5) 0.6853(4) 0.0223(13) Uani 1 1 d . . .
H3 H -0.0429 0.3909 0.7268 0.027 Uiso 1 1 calc R . .
C4 C 0.1444(10) 0.2026(5) 0.5635(4) 0.0275(15) Uani 1 1 d . . .
H4 H 0.1909 0.1538 0.5217 0.033 Uiso 1 1 calc R . .
C5 C 0.0020(8) 0.3542(5) 0.5990(4) 0.0209(13) Uani 1 1 d . . .
H5 H -0.0492 0.4106 0.5820 0.025 Uiso 1 1 calc R . .
C6 C 0.0706(8) 0.2854(5) 0.5372(4) 0.0178(12) Uani 1 1 d . . .
C7 C 0.0673(8) 0.2998(5) 0.4443(4) 0.0175(12) Uani 1 1 d . . .
C8 C 0.1940(9) 0.2670(6) 0.3908(4) 0.0282(15) Uani 1 1 d . . .
H8 H 0.2822 0.2318 0.4126 0.034 Uiso 1 1 calc R . .
C9 C -0.0623(8) 0.3480(5) 0.4094(4) 0.0220(13) Uani 1 1 d . . .
H9 H -0.1520 0.3693 0.4442 0.026 Uiso 1 1 calc R . .
C10 C 0.1938(9) 0.2847(6) 0.3060(4) 0.0281(15) Uani 1 1 d . . .
H10 H 0.2816 0.2622 0.2704 0.034 Uiso 1 1 calc R . .
C11 C -0.0643(8) 0.3658(5) 0.3244(4) 0.0204(13) Uani 1 1 d . . .
H11 H -0.1543 0.3989 0.3014 0.025 Uiso 1 1 calc R . .
C12 C 0.0653(8) 0.3350(4) 0.2741(4) 0.0161(11) Uani 1 1 d . . .
C13 C 0.5231(8) 0.0343(5) 0.2822(4) 0.0163(12) Uani 1 1 d . . .
C14A C 0.611(6) 0.109(3) 0.3506(13) 0.024(9) Uani 0.46(8) 1 d P . .
C14B C 0.668(4) 0.074(3) 0.3401(15) 0.025(5) Uani 0.54(8) 1 d P . .
C15 C 0.3943(10) -0.0343(6) 0.3035(4) 0.0349(18) Uani 1 1 d . . .
H15 H 0.3092 -0.0722 0.2597 0.042 Uiso 1 1 calc R . .
C16A C 0.602(5) 0.097(3) 0.4366(13) 0.024(8) Uani 0.46(8) 1 d P . .
C16B C 0.658(4) 0.058(3) 0.4269(12) 0.022(7) Uani 0.54(8) 1 d P . .
C17 C 0.3883(10) -0.0484(6) 0.3889(4) 0.0344(18) Uani 1 1 d . . .
H17 H 0.3001 -0.0977 0.4024 0.041 Uiso 1 1 calc R . .
C18 C 0.5051(8) 0.0063(5) 0.4541(4) 0.0204(13) Uani 1 1 d . . .
C19A C 0.504(3) 0.558(2) 0.3423(16) 0.053(7) Uiso 0.42(3) 1 d P . .
C19B C 0.518(2) 0.5142(13) 0.3533(10) 0.040(4) Uiso 0.58(3) 1 d PD . .
C20A C 0.466(3) 0.5680(19) 0.4329(13) 0.034(5) Uiso 0.42(3) 1 d P . .
C20B C 0.464(2) 0.6072(16) 0.4207(12) 0.049(5) Uiso 0.58(3) 1 d PD . .
N7B N 0.428(3) 0.667(2) 0.4824(14) 0.082(6) Uiso 0.58(3) 1 d P . .
N7A N 0.436(2) 0.6183(17) 0.4955(12) 0.041(6) Uiso 0.42(3) 1 d P . .
O1W O 0.4355(6) 0.6653(4) 0.8214(3) 0.0243(10) Uani 1 1 d D . .
H1W1 H 0.319(5) 0.675(6) 0.834(7) 0.064(16) Uiso 1 1 d D . .
H1W2 H 0.493(9) 0.734(3) 0.823(7) 0.064(16) Uiso 1 1 d D . .
O2W O 0.3946(7) 0.7339(4) 0.1463(4) 0.0354(13) Uani 1 1 d D . .
H2W1 H 0.456(9) 0.802(3) 0.166(6) 0.064(16) Uiso 1 1 d D . .
H2W2 H 0.275(4) 0.744(6) 0.150(6) 0.064(16) 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'
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
N3 Co1 N3 179.998(1) . 2_557 ?
N3 Co1 N2 89.5(2) . . ?
N3 Co1 N2 90.5(2) 2_557 . ?
N3 Co1 N2 90.5(2) . 2_557 ?
N3 Co1 N2 89.5(2) 2_557 2_557 ?
N2 Co1 N2 179.999(2) . 2_557 ?
N3 Co1 N1 89.57(19) . 2_557 ?
N3 Co1 N1 90.4(2) 2_557 2_557 ?
N2 Co1 N1 89.6(2) . 2_557 ?
N2 Co1 N1 90.4(2) 2_557 2_557 ?
N3 Co1 N1 90.4(2) . . ?
N3 Co1 N1 89.57(19) 2_557 . ?
N2 Co1 N1 90.4(2) . . ?
N2 Co1 N1 89.6(2) 2_557 . ?
N1 Co1 N1 179.999(2) 2_557 . ?
N4 Co2 N4 180.0(3) 2_667 . ?
N4 Co2 N6 88.6(2) 2_667 2_667 ?
N4 Co2 N6 91.4(2) . 2_667 ?
N4 Co2 N6 91.4(2) 2_667 . ?
N4 Co2 N6 88.6(2) . . ?
N6 Co2 N6 179.999(2) 2_667 . ?
N4 Co2 N5 90.2(2) 2_667 . ?
N4 Co2 N5 89.8(2) . . ?
N6 Co2 N5 89.6(2) 2_667 . ?
N6 Co2 N5 90.4(2) . . ?
N4 Co2 N5 89.8(2) 2_667 2_667 ?
N4 Co2 N5 90.2(2) . 2_667 ?
N6 Co2 N5 90.4(2) 2_667 2_667 ?
N6 Co2 N5 89.6(2) . 2_667 ?
N5 Co2 N5 179.999(2) . 2_667 ?
O3 S1 O1 111.4(3) . . ?
O3 S1 O2 113.7(3) . . ?
O1 S1 O2 111.7(3) . . ?
O3 S1 C1 106.3(3) . . ?
O1 S1 C1 106.8(3) . . ?
O2 S1 C1 106.4(3) . . ?
O5 S2 O6 112.4(3) . . ?
O5 S2 O4 112.3(3) . . ?
O6 S2 O4 112.3(3) . . ?
O5 S2 C12 106.5(3) . . ?
O6 S2 C12 106.1(3) . . ?
O4 S2 C12 106.6(3) . . ?
O8 S3 O7 113.8(3) . . ?
O8 S3 O9 111.4(2) . . ?
O7 S3 O9 111.9(3) . . ?
O8 S3 C13 107.8(3) . . ?
O7 S3 C13 106.2(3) . . ?
O9 S3 C13 105.1(3) . . ?
C2 C1 C3 120.2(5) . . ?
C2 C1 S1 120.1(5) . . ?
C3 C1 S1 119.6(5) . . ?
C1 C2 C4 119.8(6) . . ?
C5 C3 C1 119.4(6) . . ?
C2 C4 C6 120.7(6) . . ?
C6 C5 C3 121.5(6) . . ?
C5 C6 C4 118.4(6) . . ?
C5 C6 C7 120.7(5) . . ?
C4 C6 C7 120.9(6) . . ?
C9 C7 C8 117.8(6) . . ?
C9 C7 C6 120.5(5) . . ?
C8 C7 C6 121.7(6) . . ?
C10 C8 C7 121.2(6) . . ?
C7 C9 C11 121.5(6) . . ?
C12 C10 C8 119.4(6) . . ?
C12 C11 C9 119.2(6) . . ?
C11 C12 C10 120.8(6) . . ?
C11 C12 S2 120.0(5) . . ?
C10 C12 S2 119.2(5) . . ?
C15 C13 C14B 120.8(9) . . ?
C15 C13 C14A 116.8(10) . . ?
C14B C13 C14A 28.0(10) . . ?
C15 C13 S3 119.6(5) . . ?
C14B C13 S3 118.7(10) . . ?
C14A C13 S3 120.2(9) . . ?
C14B C14A C16A 97(3) . . ?
C14B C14A C13 75(3) . . ?
C16A C14A C13 121.0(15) . . ?
C14B C14A C16B 69(3) . . ?
C13 C14A C16B 110.2(19) . . ?
C13 C14B C16B 116.4(16) . . ?
C13 C14B C16A 107.3(17) . . ?
C13 C15 C17 120.0(6) . . ?
C16B C16A C14A 86(2) . . ?
C16B C16A C18 77(3) . . ?
C14A C16A C18 118.9(15) . . ?
C16B C16A C14B 61(2) . . ?
C18 C16A C14B 110(2) . . ?
C16A C16B C14B 93(2) . . ?
C16A C16B C18 74(3) . . ?
C14B C16B C18 121.9(12) . . ?
C16A C16B C14A 66(2) . . ?
C18 C16B C14A 110.3(13) . . ?
C18 C17 C15 122.0(6) . . ?
C17 C18 C16A 116.6(9) . . ?
C17 C18 C16B 115.7(8) . . ?
C17 C18 C18 121.9(7) . 2_656 ?
C16A C18 C18 118.8(10) . 2_656 ?
C16B C18 C18 121.0(9) . 2_656 ?
N7A C20A C19A 150(3) . . ?
C20B C20A C19B 94(3) . . ?
N7A C20A C19B 174(2) . . ?
C19A C20A N7B 121(2) . . ?
C19B C20A N7B 147(2) . . ?
C20A C20B N7B 105(3) . . ?
C20A C20B N7A 70(3) . . ?
N7B C20B C19A 168(3) . . ?
N7A C20B C19A 158(3) . . ?
N7B C20B C19B 168(2) . . ?
N7A C20B C19B 134(2) . . ?
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 N3 1.948(5) . ?
Co1 N3 1.948(5) 2_557 ?
Co1 N2 1.951(5) . ?
Co1 N2 1.951(5) 2_557 ?
Co1 N1 1.971(5) 2_557 ?
Co1 N1 1.971(5) . ?
Co2 N4 1.952(5) 2_667 ?
Co2 N4 1.952(5) . ?
Co2 N6 1.954(5) 2_667 ?
Co2 N6 1.954(5) . ?
Co2 N5 1.971(5) . ?
Co2 N5 1.971(5) 2_667 ?
S1 O3 1.456(5) . ?
S1 O1 1.458(4) . ?
S1 O2 1.459(5) . ?
S1 C1 1.777(6) . ?
S2 O5 1.456(4) . ?
S2 O6 1.456(4) . ?
S2 O4 1.459(5) . ?
S2 C12 1.789(6) . ?
S3 O8 1.455(4) . ?
S3 O7 1.457(4) . ?
S3 O9 1.471(4) . ?
S3 C13 1.766(6) . ?
C1 C2 1.382(9) . ?
C1 C3 1.388(9) . ?
C2 C4 1.385(9) . ?
C3 C5 1.384(9) . ?
C4 C6 1.398(9) . ?
C5 C6 1.379(9) . ?
C6 C7 1.501(8) . ?
C7 C9 1.384(9) . ?
C7 C8 1.391(9) . ?
C8 C10 1.389(9) . ?
C9 C11 1.394(8) . ?
C10 C12 1.377(9) . ?
C11 C12 1.372(8) . ?
C13 C15 1.369(9) . ?
C13 C14B 1.392(19) . ?
C13 C14A 1.40(2) . ?
C14A C14B 0.68(2) . ?
C14A C16A 1.39(3) . ?
C14A C16B 1.51(3) . ?
C14B C16B 1.42(2) . ?
C14B C16A 1.62(2) . ?
C15 C17 1.388(9) . ?
C16A C16B 0.710(19) . ?
C16A C18 1.41(2) . ?
C16B C18 1.428(19) . ?
C17 C18 1.363(9) . ?
C18 C18 1.484(11) 2_656 ?
C19A C19B 0.64(3) . ?
C19A C20A 1.45(3) . ?
C19A C20B 1.36(3) . ?
C19B C20A 1.42(2) . ?
C19B C20B 1.578(17) . ?
C20A C20B 0.58(2) . ?
C20A N7A 1.14(3) . ?
C20A N7B 1.46(3) . ?
C20B N7B 1.20(2) . ?
C20B N7A 1.19(2) . ?
N7B N7A 0.71(2) . ?
