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#$Date: 2016-03-26 02:12:40 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180128 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/26/7102682.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_7102682
loop_
_publ_author_name
'Turner, David R'
'Hursthouse, M B'
'Light, M E'
'Steed, Jonathan W'
_publ_section_title
;
 Linear distortion of octahedral metal centres by multiple hydrogen
 bonds in modular ML(4) systems.
;
_journal_issue                   12
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1354
_journal_page_last               1355
_journal_paper_doi               10.1039/b402884h
_journal_year                    2004
_chemical_formula_sum            'C52 H64 Co N12 O12 S'
_chemical_formula_weight         1140.14
_chemical_name_systematic
;
?
;
_space_group_IT_number           85
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.070(3)
_cell_length_b                   18.070(3)
_cell_length_c                   8.0756(16)
_cell_measurement_temperature    173(2)
_cell_volume                     2636.9(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            4642
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    0.440
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1198
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       0.018(2)
_refine_ls_extinction_expression Fc^*^==kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         3007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0429
_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)+(0.0000P)²+4.2991P] where P==(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1018
_reflns_number_gt                2864
_reflns_number_total             3007
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b402884h.txt
_cod_data_source_block           c:\dave\structs\dtheat\dtco1\dtco1
_cod_database_code               7102682
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/2, x, z'
'-x+1/2, -y+1/2, z'
'y, -x+1/2, z'
'-x, -y, -z'
'y-1/2, -x, -z'
'x-1/2, y-1/2, -z'
'-y, x-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
Co1 Co 0.2500 0.2500 0.23627(6) 0.00996(16) Uani 1 4 d S . .
S1 S 0.2500 0.7500 0.5000 0.0117(2) Uani 1 4 d S . .
N2 N 0.22515(10) 0.53611(9) 0.4829(2) 0.0172(4) Uani 1 1 d . A .
H2 H 0.2258 0.5838 0.4610 0.021 Uiso 1 1 calc R . .
C8 C 0.16345(11) 0.63216(11) 0.9966(3) 0.0164(4) Uani 1 1 d . . .
H8 H 0.1923 0.6724 0.9568 0.020 Uiso 1 1 calc R . .
O2 O 0.2500 0.2500 -0.0272(4) 0.0153(5) Uani 1 4 d S . .
N1 N 0.26772(9) 0.36859(8) 0.2353(2) 0.0135(3) Uani 1 1 d . . .
O1 O 0.2500 0.2500 0.4935(3) 0.0166(6) Uani 1 4 d S . .
C11 C 0.08213(14) 0.51518(13) 1.1171(3) 0.0274(5) Uani 1 1 d . . .
H11 H 0.0551 0.4741 1.1587 0.033 Uiso 1 1 calc R . .
C10 C 0.09022(12) 0.57733(12) 1.2161(3) 0.0211(4) Uani 1 1 d . . .
C9 C 0.13253(11) 0.63561(11) 1.1537(3) 0.0187(4) Uani 1 1 d . . .
H9 H 0.1403 0.6784 1.2199 0.022 Uiso 1 1 calc R . .
C13 C 0.05267(14) 0.58227(15) 1.3829(3) 0.0310(5) Uani 1 1 d . . .
H13A H 0.0006 0.5957 1.3675 0.047 Uiso 1 1 calc R . .
H13B H 0.0773 0.6200 1.4503 0.047 Uiso 1 1 calc R . .
H13C H 0.0558 0.5343 1.4389 0.047 Uiso 1 1 calc R . .
C7 C 0.15259(11) 0.57032(11) 0.8968(3) 0.0168(4) Uani 1 1 d . . .
C12 C 0.11219(14) 0.51083(12) 0.9592(3) 0.0270(5) Uani 1 1 d . . .
H12 H 0.1053 0.4676 0.8942 0.032 Uiso 1 1 calc R . .
O4 O 0.28082(8) 0.68991(8) 0.3966(2) 0.0221(3) Uani 1 1 d . . .
C5 C 0.23867(10) 0.41226(10) 0.3539(2) 0.0149(4) Uani 1 1 d . . .
H5 H 0.2086 0.3904 0.4371 0.018 Uiso 1 1 calc R . .
C2 C 0.31997(13) 0.47570(12) 0.1071(3) 0.0238(5) Uani 1 1 d . . .
H2A H 0.3474 0.4966 0.0183 0.029 Uiso 1 1 calc R . .
C1 C 0.30854(12) 0.39981(11) 0.1153(3) 0.0197(4) Uani 1 1 d . . .
H1 H 0.3303 0.3690 0.0333 0.024 Uiso 1 1 calc R . .
N3 N 0.18073(10) 0.57378(9) 0.7333(2) 0.0174(4) Uani 1 1 d . A .
H3 H 0.1871 0.6182 0.6912 0.021 Uiso 1 1 calc R . .
C3 C 0.29109(12) 0.52031(11) 0.2295(3) 0.0207(4) Uani 1 1 d . . .
H3A H 0.2984 0.5723 0.2257 0.025 Uiso 1 1 calc R . .
C4 C 0.25114(11) 0.48866(10) 0.3587(2) 0.0152(4) Uani 1 1 d . . .
C6 C 0.19884(14) 0.51567(11) 0.6350(3) 0.0248(5) Uani 1 1 d . . .
O3A O 0.2079(2) 0.4513(3) 0.6895(6) 0.0190(9) Uani 0.50 1 d P A 1
O5 O 0.30608(15) 0.34063(15) 0.7292(3) 0.0158(5) Uani 0.50 1 d P . .
O3B O 0.1748(3) 0.4508(3) 0.6627(6) 0.0305(11) Uani 0.50 1 d P A 2
H2O H 0.2811 0.2261 -0.0987 0.23(4) Uiso 1 1 d R . .
H1O H 0.2632 0.2831 0.5689 0.43(6) Uiso 1 1 d R . .
H4 H 0.3557 0.3475 0.7187 0.010(11) Uiso 0.50 1 d PR . .
H6 H 0.2831 0.3769 0.7630 0.06(2) Uiso 0.50 1 d PR . .
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
O1 Co1 O2 180.000(1) . .
O1 Co1 N1 90.21(5) . 3
O2 Co1 N1 89.79(5) . 3
O1 Co1 N1 90.21(5) . .
O2 Co1 N1 89.79(5) . .
N1 Co1 N1 179.59(9) 3 .
O1 Co1 N1 90.21(5) . 2
O2 Co1 N1 89.79(5) . 2
N1 Co1 N1 89.999(1) 3 2
N1 Co1 N1 89.999(1) . 2
O1 Co1 N1 90.21(5) . 4
O2 Co1 N1 89.79(5) . 4
N1 Co1 N1 89.999(1) 3 4
N1 Co1 N1 89.999(1) . 4
N1 Co1 N1 179.59(9) 2 4
O4 S1 O4 108.59(6) 8_666 .
O4 S1 O4 111.25(13) 8_666 6_566
O4 S1 O4 108.59(6) . 6_566
O4 S1 O4 108.59(6) 8_666 3_565
O4 S1 O4 111.25(13) . 3_565
O4 S1 O4 108.59(6) 6_566 3_565
C6 N2 C4 126.47(17) . .
C9 C8 C7 120.59(19) . .
C1 N1 C5 118.76(16) . .
C1 N1 Co1 119.96(13) . .
C5 N1 Co1 121.28(13) . .
C10 C11 C12 122.3(2) . .
C11 C10 C9 117.5(2) . .
C11 C10 C13 121.0(2) . .
C9 C10 C13 121.5(2) . .
C8 C9 C10 121.10(19) . .
C8 C7 C12 118.91(19) . .
C8 C7 N3 116.99(18) . .
C12 C7 N3 124.03(18) . .
C11 C12 C7 119.6(2) . .
N1 C5 C4 122.33(18) . .
C3 C2 C1 119.17(19) . .
N1 C1 C2 122.07(19) . .
C6 N3 C7 126.74(18) . .
C2 C3 C4 119.59(18) . .
C3 C4 C5 117.92(18) . .
C3 C4 N2 117.34(17) . .
C5 C4 N2 124.73(18) . .
O3A C6 O3B 29.2(2) . .
O3A C6 N3 123.0(3) . .
O3B C6 N3 121.9(3) . .
O3A C6 N2 121.3(3) . .
O3B C6 N2 121.8(3) . .
N3 C6 N2 113.60(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1 2.077(3) .
Co1 O2 2.127(3) .
Co1 N1 2.1667(16) 3
Co1 N1 2.1667(16) .
Co1 N1 2.1667(16) 2
Co1 N1 2.1667(16) 4
S1 O4 1.4786(14) 8_666
S1 O4 1.4786(14) .
S1 O4 1.4786(14) 6_566
S1 O4 1.4786(14) 3_565
N2 C6 1.368(3) .
N2 C4 1.401(2) .
C8 C9 1.388(3) .
C8 C7 1.392(3) .
N1 C1 1.343(3) .
N1 C5 1.347(2) .
C11 C10 1.386(3) .
C11 C12 1.388(3) .
C10 C9 1.395(3) .
C10 C13 1.511(3) .
C7 C12 1.394(3) .
C7 N3 1.416(3) .
C5 C4 1.399(3) .
C2 C3 1.378(3) .
C2 C1 1.388(3) .
N3 C6 1.357(3) .
C3 C4 1.391(3) .
C6 O3A 1.255(5) .
C6 O3B 1.270(5) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2 O4 0.88 2.22 3.037(2) 154.0 .
N3 H3 O4 0.88 1.96 2.834(2) 173.7 6_566
O2 H2O O5 0.92 1.85 2.753(3) 168.4 4_554
O1 H1O O5 0.89 1.83 2.708(3) 169.3 .
O5 H4 O3B 0.91 1.82 2.685(6) 157.4 4
O5 H4 O3A 0.91 2.01 2.785(5) 142.2 4
O5 H6 O3B 0.82 2.51 3.144(6) 135.4 .
O5 H6 O3A 0.82 2.00 2.691(5) 141.2 .
