#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2003054.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2003054
loop_
_publ_author_name
'Zhou, Ping'
'Xue, Feng'
'Au-Yeung, Steve C. F.'
'Xu, Xiao-ping'
_publ_section_title
;
 Crystal structures of [18]aneN~6~H~2~K[Co(CN)~6~].4H~2~O,
 [16]aneN~4~H~2~K[Co(CN)~6~] and [12]aneN~4~H~3~[Co(CN)~6~].2H~2~O.
 Insight into the electrostatic and hydrogen-bonding interaction in
 self-assembling supercomplexes
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              389
_journal_page_last               395
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          'K H2[Co(C N)6](C12 H30 N6).4(H2 O)'
_chemical_formula_moiety         'C18 H32 Co K N12,4(H2 O)'
_chemical_formula_sum            'C18 H40 Co K N12 O4'
_chemical_formula_weight         586.65
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                73.780(10)
_cell_angle_beta                 71.680(10)
_cell_angle_gamma                68.87(2)
_cell_formula_units_Z            2
_cell_length_a                   10.125(3)
_cell_length_b                   11.133(2)
_cell_length_c                   15.014(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      5
_cell_volume                     1472.0(6)
_computing_cell_refinement       'Siemens XSCANS ver. 2.10b'
_computing_data_collection       'Siemens XSCANS ver. 2.10b'
_computing_data_reduction        'Siemens XSCANS ver. 2.10b'
_computing_molecular_graphics    'SHELXTL-PC (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0340
_diffrn_reflns_av_sigmaI/netI    .0851
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4910
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.45
_diffrn_standards_decay_%        -1.25
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .769
_exptl_absorpt_correction_T_max  .946
_exptl_absorpt_correction_T_min  .833
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       Plate
_exptl_crystal_F_000             620
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .10
_refine_diff_density_max         .360
_refine_diff_density_min         -.620
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.38
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         3023
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .0964
_refine_ls_R_factor_obs          .0592
_refine_ls_shift/esd_max         .001
_refine_ls_shift/esd_mean        .000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      'calc w=1/[\s^2^(Fo)+0.0005Fo^2^]'
_refine_ls_wR_factor_all         .0745
_refine_ls_wR_factor_obs         .0667
_reflns_number_observed          3032
_reflns_number_total             4617
_reflns_observed_criterion       >4sigma(F)
_[local]_cod_data_source_file    oa0016.cif
_[local]_cod_data_source_block   1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2003054
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Co1 .0260(10) .0260(10) .0230(10) -.0040(10) -.0050(10) -.0100(10)
C1 .028(4) .034(4) .041(4) -.007(3) -.014(3) -.003(3)
N1 .045(4) .042(3) .062(4) .001(3) -.013(3) -.027(3)
C2 .045(4) .040(4) .030(4) -.009(3) -.003(3) -.017(4)
N2 .072(5) .060(4) .046(4) -.03(3) .003(3) -.036(4)
C3 .038(4) .030(4) .043(4) -.004(3) -.009(3) -.017(3)
N3 .045(4) .044(4) .067(4) -.010(3) -.016(3) -.004(3)
C4 .036(4) .034(4) .040(4) -.006(3) -.005(3) -.013(3)
N4 .061(4) .068(4) .036(4) -.016(3) -.013(3) -.017(3)
C5 .042(4) .042(4) .024(3) -.006(3) -.010(3) -.016(4)
N5 .035(4) .060(4) .048(4) -.015(3) -.016(3) .004(3)
C6 .040(4) .040(4) .036(4) -.005(3) -.014(3) -.009(3)
N6 .086(5) .060(4) .051(4) -.012(3) -.033(4) -.022(4)
K1 .0590(10) .0690(10) .0400(10) -.0070(10) -.0080(10) -.0240(10)
N11 .031(3) .046(3) .039(3) -.003(3) -.010(2) -.012(3)
N12 .046(4) .042(3) .045(3) -.008(3) -.012(3) -.010(3)
N13 .040(3) .037(3) .038(3) -.006(2) -.011(3) -.019(3)
C11 .029(4) .053(4) .046(4) -.011(3) -.007(3) -.012(3)
C12 .032(4) .039(4) .060(5) -.006(3) -.008(3) -.004(3)
C13 .053(5) .040(4) .046(4) -.013(3) -.003(4) -.006(4)
C14 .053(5) .028(4) .066(5) -.006(3) -.019(4) -.014(3)
C15 .058(5) .039(4) .044(4) .000(3) -.011(4) -.025(4)
C16 .036(4) .052(4) .039(4) -.012(3) -.001(3) -.023(3)
N21 .055(4) .046(3) .055(4) -.015(3) -.010(3) -.021(3)
N22 .065(4) .040(3) .058(4) -.008(3) -.029(3) -.023(3)
N23 .036(3) .052(4) .047(3) -.004(3) -.017(3) -.018(3)
C21 .048(5) .048(4) .077(6) -.023(4) -.009(4) -.012(4)
C22 .077(6) .048(5) .063(5) -.027(4) -.005(4) -.021(4)
C23 .073(6) .046(4) .053(5) -.012(4) -.022(4) -.022(4)
C24 .072(5) .054(5) .039(4) -.03(3) -.021(4) -.031(4)
C25 .076(5) .061(5) .036(4) -.003(3) -.025(4) -.034(4)
C26 .053(5) .044(4) .066(5) .001(4) -.020(4) -.016(4)
O1W .063(4) .129(6) .105(5) .050(4) -.033(4) -.036(4)
O2W .116(6) .113(6) .141(6) .004(5) -.033(5) -.083(5)
O3W .069(4) .114(5) .089(4) -.046(4) -.021(4) .016(4)
O4W .153(8) .115(6) .164(8) -.020(6) -.063(6) -.029(6)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Co1 .26070(10) .27640(10) .28940(10) .0250(10) Uani d . 1 Co
C1 .1670(7) .1451(6) .3620(4) .035(3) Uani d . 1 C
N1 .1076(6) .0702(5) .4054(4) .048(3) Uani d . 1 N
C2 .3494(7) .4107(6) .2223(4) .038(3) Uani d . 1 C
N2 .3998(7) .4926(6) .1854(4) .061(3) Uani d . 1 N
C3 .0782(7) .4080(6) .3063(4) .036(3) Uani d . 1 C
N3 -.0325(7) .4876(6) .3142(4) .054(3) Uani d . 1 N
C4 .2940(7) .2896(6) .4040(5) .037(3) Uani d . 1 C
N4 .3185(7) .2939(6) .4724(4) .054(3) Uani d . 1 N
C5 .4467(7) .1490(6) .2665(4) .035(3) Uani d . 1 C
N5 .5575(6) .0730(6) .2514(4) .050(3) Uani d . 1 N
C6 .2325(7) .2547(6) .1756(5) .038(3) Uani d . 1 C
N6 .2167(7) .2382(6) .1083(4) .061(3) Uani d . 1 N
K1 -.0057(2) -.0181(2) .12730(10) .0560(10) Uani d . 1 K
N11 -.2878(5) .1178(5) .0404(4) .039(2) Uani d . 1 N
H11M -.1964 .1003 .0034 .050 Uiso d R 1 H
H11N -.2855 .0906 .1024 .050 Uiso d R .5 H
N12 -.1567(6) .3214(5) -.0442(4) .045(3) Uani d . 1 N
H12M -.1919 .3493 -.0969 .050 Uiso d R 1 H
N13 .1399(5) .1870(5) -.0389(3) .036(2) Uani d . 1 N
H13M .1504 .1848 .0201 .050 Uiso d R 1 H
H13N .0752 .1494 -.0491 .050 Uiso d R .5 H
C11 -.3514(7) .0193(6) .0349(5) .043(3) Uani d . 1 C
H11A -.3322 .0144 -.0310 .060 Uiso d R 1 H
H11B -.4552 .0487 .0589 .060 Uiso d R 1 H
C12 -.3747(7) .2553(6) .0151(5) .047(3) Uani d . 1 C
H12A -.4701 .2709 .0573 .060 Uiso d R 1 H
H12B -.3850 .2713 -.0490 .060 Uiso d R 1 H
C13 -.2992(8) .3453(7) .0214(5) .050(3) Uani d . 1 C
H13A -.3567 .4351 .0073 .060 Uiso d R 1 H
H13B -.2857 .3278 .0848 .060 Uiso d R 1 H
C14 -.0642(7) .3888(6) -.0356(5) .048(3) Uani d . 1 C
H14A -.0682 .3776 .0309 .060 Uiso d R 1 H
H14B -.0962 .4809 -.0609 .060 Uiso d R 1 H
C15 .0901(8) .3273(6) -.0866(5) .046(3) Uani d . 1 C
H15A .0925 .3316 -.1518 .060 Uiso d R 1 H
H15B .1538 .3732 -.0859 .060 Uiso d R 1 H
C16 .2899(7) .1173(6) -.0884(4) .041(3) Uani d . 1 C
H16A .3534 .1688 -.0984 .060 Uiso d R 1 H
H16B .2868 .1098 -.1498 .060 Uiso d R 1 H
N21 .1576(6) -.3043(5) .4705(4) .050(3) Uani d . 1 N
H21M .1216 -.3646 .5156 .060 Uiso d R 1 H
N22 -.0101(7) -.1100(5) .3476(4) .049(3) Uani d . 1 N
H22M .0417 -.0901 .3773 .060 Uiso d R 1 H
N23 -.2200(6) .1586(5) .4304(4) .043(3) Uani d . 1 N
H23M -.1322 .1403 .4422 .050 Uiso d R 1 H
H23N -.3041 .1493 .4709 .050 Uiso d R 1 H
C21 .2979(8) -.3494(7) .4924(6) .057(4) Uani d . 1 C
H21A .3355 -.4431 .5000 .080 Uiso d R 1 H
H21B .3640 -.3122 .4402 .080 Uiso d R 1 H
C22 .1608(9) -.3290(7) .3774(5) .061(4) Uani d . 1 C
H22A .2365 -.3001 .3285 .080 Uiso d R 1 H
H22B .1804 -.4209 .3806 .080 Uiso d R 1 H
C23 .0202(8) -.2534(6) .3533(5) .054(4) Uani d . 1 C
H23A -.0551 -.2829 .4022 .080 Uiso d R 1 H
H23B .0186 -.2674 .2934 .080 Uiso d R 1 H
C24 -.1668(8) -.0391(7) .3622(5) .050(4) Uani d . 1 C
H24A -.2034 -.0627 .3199 .080 Uiso d R 1 H
H24B -.2166 -.0667 .4265 .080 Uiso d R 1 H
C25 -.2009(9) .1085(7) .3438(5) .052(4) Uani d . 1 C
H25A -.2880 .1499 .3206 .080 Uiso d R 1 H
H25B -.1218 .1320 .2951 .080 Uiso d R 1 H
C26 -.2851(8) .3060(7) .4179(5) .055(4) Uani d . 1 C
H26A -.3797 .3314 .4053 .080 Uiso d R 1 H
H26B -.2242 .3473 .3646 .080 Uiso d R 1 H
O1W .5410(6) .0953(7) .5561(4) .109(4) Uani d . 1 O
H1WA .4748 .1553 .5318 .100 Uiso d R 1 H
H1WB .5514 .0486 .5168 .100 Uiso d R 1 H
O2W .5361(7) .6723(7) .2006(5) .115(5) Uani d . 1 O
H2WA .4972 .6191 .1956 .120 Uiso d R 1 H
H2WB .4752 .7100 .2456 .120 Uiso d R 1 H
O3W -.3176(6) .6593(6) .3319(4) .097(4) Uani d . 1 O
H3WA -.2313 .6072 .3261 .100 Uiso d R 1 H
H3WB -.3374 .6901 .3819 .100 Uiso d R 1 H
O4W .3133(9) .9111(7) .2125(6) .142(6) Uani d . 1 O
H4WA .2233 .9258 .2404 .150 Uiso d R 1 H
H4WB .3860 .8558 .2328 .150 Uiso d R 1 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K .2009 .2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co .3494 .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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 Co1 C2 . . 177.3(3) yes
C1 Co1 C3 . . 90.1(3) yes
C2 Co1 C3 . . 88.4(3) yes
C1 Co1 C4 . . 89.1(3) yes
C2 Co1 C4 . . 88.8(3) yes
C3 Co1 C4 . . 92.3(3) yes
C1 Co1 C5 . . 92.2(3) yes
C2 Co1 C5 . . 89.4(3) yes
C3 Co1 C5 . . 177.3(2) yes
C4 Co1 C5 . . 89.2(3) yes
C1 Co1 C6 . . 89.6(3) yes
C2 Co1 C6 . . 92.6(3) yes
C3 Co1 C6 . . 90.0(3) yes
C4 Co1 C6 . . 177.3(2) yes
C5 Co1 C6 . . 88.5(3) yes
Co1 C1 N1 . . 177.9(5) yes
Co1 C2 N2 . . 177.4(6) yes
Co1 C3 N3 . . 178.1(7) yes
Co1 C4 N4 . . 177.5(5) yes
Co1 C5 N5 . . 178.9(6) yes
Co1 C6 N6 . . 178.2(6) yes
N11 K1 N13 . . 86.10(10) no
N11 K1 N22 . . 125.40(10) no
N13 K1 N22 . . 131.7(2) no
N11 K1 C24 . . 99.9(2) no
N13 K1 C24 . . 136.1(2) no
N22 K1 C24 . . 25.8(2) no
N11 K1 K1 . 2 56.50(10) no
N13 K1 K1 . 2 58.00(10) no
N22 K1 K1 . 2 168.20(10) no
C24 K1 K1 . 2 154.8(2) no
N11 K1 N11 . 2 110.70(10) no
N13 K1 N11 . 2 58.10(10) no
N22 K1 N11 . 2 122.30(10) no
C24 K1 N11 . 2 147.9(2) no
K1B K1 N11 . 2 54.20(10) no
N11 K1 N13 . 2 57.60(10) no
N13 K1 N13 . 2 112.30(10) no
N22 K1 N13 . 2 115.5(2) no
C24 K1 N13 . 2 107.3(2) no
K1 K1 N13 2 2 54.30(10) no
N11 K1 N13 2 2 82.40(10) no
K1 N11 C11 . . 111.8(3) no
K1 N11 C12 . . 133.5(5) no
C11 N11 C12 . . 114.4(6) no
K1 N11 K1 . 2 69.30(10) no
C11 N11 K1 . 2 92.1(3) no
C12 N11 K1 . 2 114.0(3) no
C13 N12 C14 . . 114.7(6) no
K1 N13 C15 . . 136.8(3) no
K1 N13 C16 . . 110.4(3) no
C15 N13 C16 . . 112.2(4) no
K1 N13 K1 . 2 67.70(10) no
C15 N13 K1 . 2 106.2(5) no
C16 N13 K1 . 2 88.9(4) no
N11 C11 C16 . 2 114.0(6) no
N11 C12 C13 . . 109.7(6) no
N12 C13 C12 . . 109.1(6) no
N12 C14 C15 . . 108.6(6) no
N13 C15 C14 . . 109.0(5) no
N13 C16 C11 . 2 113.5(5) no
C21 N21 C22 . . 114.1(6) no
K1 N22 C23 . . 97.7(4) no
K1 N22 C24 . . 84.8(4) no
C23 N22 C24 . . 112.1(6) no
C25 N23 C26 . . 112.5(5) no
N21 C21 C26 . 2 109.7(6) no
N21 C22 C23 . . 108.7(6) no
N22 C23 C22 . . 111.0(8) no
K1 C24 N22 . . 69.5(3) no
K1 C24 C25 . . 86.2(3) no
N22 C24 C25 . . 113.9(7) no
N23 C25 C24 . . 112.7(5) no
N23 C26 C21 . 2 109.3(6) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 C1 . 1.920(7) yes
Co1 C2 . 1.901(7) yes
Co1 C3 . 1.894(6) yes
Co1 C4 . 1.909(8) yes
Co1 C5 . 1.902(6) yes
Co1 C6 . 1.909(8) yes
C1 N1 . 1.137(9) yes
C2 N2 . 1.129(10) yes
C3 N3 . 1.147(8) yes
C4 N4 . 1.146(11) yes
C5 N5 . 1.135(8) yes
C6 N6 . 1.143(11) yes
K1 N11 . 3.205(6) yes
K1 N13 . 3.247(5) yes
K1 N22 . 3.168(6) yes
K1 C24 . 3.369(7) yes
K1 K1 2 3.699(4) yes
K1 N11 2 3.298(5) yes
K1 N13 2 3.393(7) yes
N11 C11 . 1.489(11) yes
N11 C12 . 1.475(7) yes
N11 K1 2 3.298(5) yes
N12 C13 . 1.449(8) yes
N12 C14 . 1.447(11) yes
N13 C15 . 1.496(7) yes
N13 C16 . 1.492(7) yes
N13 K1 2 3.393(7) yes
C11 C16 2 1.514(8) yes
C12 C13 . 1.500(13) yes
C14 C15 . 1.505(9) yes
C16 C11 2 1.514(8) yes
N21 C21 . 1.437(11) yes
N21 C22 . 1.486(11) yes
N22 C23 . 1.496(9) yes
N22 C24 . 1.471(9) yes
N23 C25 . 1.486(10) yes
N23 C26 . 1.513(8) yes
C21 C26 2_556 1.508(13) yes
C22 C23 . 1.469(11) yes
C24 C25 . 1.513(10) yes
C26 C21 2_556 1.508(13) yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
N22 N1 3.089(9) . . no
O2W N2 2.898(9) . . no
O1W N4 2.860(9) . . no
N13 N6 2.814(9) . . no
O2W O4W 2.807(9) . . no
N23 N1 3.030(9) . . no
O3W N3 2.807(9) . . no
N11 N5 3.049(9) 1_655 . no
O1W N23 2.745(9) . 1_655 no
O2W O3W 2.761(9) . 1_655 no