#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2003055.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_2003055
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 H28 N4)'
_chemical_formula_moiety         'C18 H30 Co K N10'
_chemical_formula_sum            'C18 H30 Co K N10'
_chemical_formula_weight         484.55
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 91.89(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.675(2)
_cell_length_b                   10.516(2)
_cell_length_c                   21.051(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      5
_cell_volume                     2361.9(8)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'MSC/AFC Diffractometer Control'
_computing_molecular_graphics    'SHELXTL-PC (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXTL-PC (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source
;
Rigaku RU-200 rotating-anode generator powered at 50kV and 90mA
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0211
_diffrn_reflns_av_sigmaI/netI    .0998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            5713
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        -1.72
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .928
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  .942
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_description       Block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .22
_refine_diff_density_max         .310
_refine_diff_density_min         -.690
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.62
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3133
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .1070
_refine_ls_R_factor_obs          .0489
_refine_ls_shift/esd_max         .082
_refine_ls_shift/esd_mean        .004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      'calc w=1/[\s^2^(Fo)+0.0002Fo^2^]'
_refine_ls_wR_factor_all         .0625
_refine_ls_wR_factor_obs         .0582
_reflns_number_observed          3133
_reflns_number_total             5425
_reflns_observed_criterion       >4sigma(F)
_[local]_cod_data_source_file    oa0016.cif
_[local]_cod_data_source_block   2
_[local]_cod_cif_authors_sg_H-M  'P 21/c'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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               2003055
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_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
K(1) .0500(10) .0390(10) .0610(10) .0030(10) .0080(10) .0010(10)
Co(1) .0250(10) .0210(10) .0270(10) -.0050(10) .0020(10) .0000(10)
C(1) .0320(10) .0330(10) .0360(10) -.0070(10) -.0030(10) .0010(10)
N(1) .0510(10) .0360(10) .0740(10) -.0210(10) -.0010(10) .0000(10)
C(2) .0270(10) .0250(10) .0390(10) -.0050(10) .0020(10) -.0030(10)
N(2) .0450(10) .0470(10) .0380(10) .0050(10) .0020(10) -.0030(10)
C(3) .0340(10) .0300(10) .0290(10) .0040(10) .0040(10) -.0010(10)
N(3) .0650(10) .0310(10) .0550(10) -.0110(10) .0030(10) -.0090(10)
C(4) .0280(10) .0280(10) .0390(10) -.0100(10) .0010(10) -.0010(10)
N(4) .0520(10) .0470(10) .0300(10) -.0010(10) .0010(10) -.0020(10)
C(5) .0370(10) .0340(10) .0260(10) -.0050(10) .0050(10) .0030(10)
N(5) .0360(10) .0680(10) .0460(10) -.0040(10) .0060(10) .0150(10)
C(6) .0330(10) .0260(10) .0320(10) .0000(10) .0010(10) -.0020(10)
N(6) .0280(10) .0410(10) .0470(10) -.0020(10) .0080(10) .0000(10)
N(7) .0360(10) .0310(10) .0250(10) -.0020(10) .0020(10) -.0050(10)
N(8) .0280(10) .0370(10) .0510(10) -.0090(10) .0020(10) -.0050(10)
N(9) .0390(10) .0410(10) .0310(10) .0080(10) .0090(10) .0080(10)
N(10) .0310(10) .0480(10) .0380(10) -.0020(10) .0020(10) -.0080(10)
C(7) .0400(10) .0330(10) .0330(10) -.0070(10) .0000(10) -.0070(10)
C(8) .0350(10) .0250(10) .0420(10) .0040(10) .0050(10) -.0040(10)
C(9) .0350(10) .0330(10) .0410(10) .0040(10) .0000(10) -.0010(10)
C(10) .0470(10) .0320(10) .0480(10) -.0060(10) .0140(10) -.0080(10)
C(11) .0480(10) .0340(10) .0450(10) -.0010(10) -.0010(10) .0010(10)
C(12) .0490(10) .0360(10) .0430(10) .0040(10) .0100(10) .0030(10)
C(13) .0390(10) .0370(10) .0360(10) -.0040(10) .0040(10) .0000(10)
C(14) .0340(10) .0340(10) .0410(10) -.0020(10) .0070(10) .0030(10)
C(15) .0420(10) .0350(10) .0350(10) -.0030(10) .0040(10) -.0050(10)
C(16) .0310(10) .0450(10) .0420(10) -.0110(10) .0000(10) .0020(10)
C(17) .0430(10) .0440(10) .0420(10) .0020(10) -.0030(10) -.0040(10)
C(18) .0490(10) .0430(10) .0510(10) .0090(10) -.0160(10) -.0060(10)
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
K1 .18830(10) .48270(10) -.12280(10) .0500(10) Uani d . 1 K
Co1 .27730(10) .79670(10) .11540(10) .0240(10) Uani d . 1 Co
C1 .2340(3) .6309(3) .0861(2) .0340(10) Uani d . 1 C
N1 .2133(3) .5307(3) .0676(2) .0540(10) Uani d . 1 N
C2 .2784(3) .7396(3) .2007(2) .0300(10) Uani d . 1 C
N2 .2797(3) .7090(3) .2528(2) .0430(10) Uani d . 1 N
C3 .3258(3) .9590(3) .1457(2) .0310(10) Uani d . 1 C
N3 .3537(3) 1.0568(3) .1662(2) .0500(10) Uani d . 1 N
C4 .2689(3) .8551(3) .0294(2) .0320(10) Uani d . 1 C
N4 .2573(3) .8862(3) -.0228(2) .0430(10) Uani d . 1 N
C5 .4495(3) .7521(3) .1106(2) .0320(10) Uani d . 1 C
N5 .5526(3) .7239(3) .1106(2) .0500(10) Uani d . 1 N
C6 .1073(3) .8442(3) .1248(2) .0310(10) Uani d . 1 C
N6 .0073(3) .8767(3) .1333(2) .0390(10) Uani d . 1 N
N7 .2863(3) .3083(3) -.0036(2) .0310(10) Uani d . 1 N
H(7) .2496 .3735 .0163 .050 Uiso d R 1 H
H(7N) .3238 .3241 -.0405 .050 Uiso d PR .5 H
N8 -.0723(3) .2521(3) .1003(2) .0390(10) Uani d . 1 N
H(8) -.1264 .1966 .0818 .050 Uiso d R 1 H
H(8N) -.1253 .3173 .1060 .050 Uiso d PR .5 H
N9 .1996(3) .2945(3) .2989(2) .0370(10) Uani d . 1 N
H(9) .2369 .2500 .3308 .050 Uiso d R 1 H
H(9N) .1315 .3148 .3208 .050 Uiso d PR .5 H
N10 .5733(3) .3938(3) .1733(2) .0390(10) Uani d . 1 N
H(10) .6145 .4637 .1608 .050 Uiso d R 1 H
H(10N) .6226 .3490 .2006 .050 Uiso d PR .5 H
C7 .1846(3) .2164(3) -.0234(2) .0350(10) Uani d . 1 C
H(7A) .2233 .1414 -.0399 .100 Uiso d R 1 H
H(7B) .1345 .2538 -.0572 .100 Uiso d R 1 H
C8 .0981(3) .1784(3) .0293(2) .0340(10) Uani d . 1 C
H(8A) .1481 .1482 .0649 .100 Uiso d R 1 H
H(8B) .0441 .1105 .0151 .100 Uiso d R 1 H
C9 .0189(3) .2885(3) .0505(2) .0370(10) Uani d . 1 C
H(9A) .0730 .3539 .0675 .100 Uiso d R 1 H
H(9B) -.0260 .3226 .0141 .100 Uiso d R 1 H
C10 -.0193(3) .1949(3) .1598(2) .0420(10) Uani d . 1 C
H(10A) .0311 .1226 .1496 .100 Uiso d R 1 H
H(10B) -.0862 .1658 .1855 .100 Uiso d R 1 H
C11 .0614(3) .2887(3) .1987(2) .0420(10) Uani d . 1 C
H(11A) .0097 .3523 .2174 .100 Uiso d R 1 H
H(11B) .1201 .3298 .1718 .100 Uiso d R 1 H
C12 .1301(3) .2131(3) .2505(2) .0420(10) Uani d . 1 C
H(12A) .0705 .1608 .2715 .100 Uiso d R 1 H
H(12B) .1889 .1577 .2308 .100 Uiso d R 1 H
C13 .2822(3) .3959(3) .2744(2) .0370(10) Uani d . 1 C
H(13A) .3186 .4436 .3092 .100 Uiso d R 1 H
H(13B) .2326 .4530 .2484 .100 Uiso d R 1 H
C14 .3870(3) .3410(3) .2350(2) .0360(10) Uani d . 1 C
H(14A) .3513 .2857 .2030 .100 Uiso d R 1 H
H(14B) .4427 .2919 .2620 .100 Uiso d R 1 H
C15 .4606(3) .4460(3) .2040(2) .0370(10) Uani d . 1 C
H(15A) .4078 .4870 .1724 .100 Uiso d R 1 H
H(15B) .4850 .5081 .2354 .100 Uiso d R 1 H
C16 .5530(3) .2978(3) .1215(2) .0390(10) Uani d . 1 C
H(16A) .5089 .2265 .1385 .100 Uiso d R 1 H
H(16B) .6326 .2681 .1076 .100 Uiso d R 1 H
C17 .4772(3) .3494(3) .0643(2) .0430(10) Uani d . 1 C
H(17A) .5310 .3653 .0295 .100 Uiso d R 1 H
H(17B) .4385 .4281 .0760 .100 Uiso d R 1 H
C18 .3773(3) .2554(3) .0448(2) .0480(10) Uani d . 1 C
H(18A) .4167 .1815 .0276 .100 Uiso d R 1 H
H(18B) .3330 .2298 .0817 .100 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'
Co Co .3494 .9721 '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'
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
N7 K1 N8 . 3_565 120.60(10) no
N7 K1 N9 . 4_565 82.70(10) no
N8 K1 N9 3_565 4_565 151.70(10) no
N7 K1 N10 . 3_665 104.80(10) no
N8 K1 N10 3_565 3_665 90.70(10) no
N9 K1 N10 4_565 3_665 98.80(10) no
C1 Co1 C2 . . 90.6(2) yes
C1 Co1 C3 . . 177.90(10) yes
C2 Co1 C3 . . 88.4(2) yes
C1 Co1 C4 . . 89.2(2) yes
C2 Co1 C4 . . 177.70(10) yes
C3 Co1 C4 . . 91.9(2) yes
C1 Co1 C5 . . 89.00(10) yes
C2 Co1 C5 . . 89.8(2) yes
C3 Co1 C5 . . 89.20(10) yes
C4 Co1 C5 . . 92.6(2) yes
C1 Co1 C6 . . 93.00(10) yes
C2 Co1 C6 . . 87.7(2) yes
C3 Co1 C6 . . 88.80(10) yes
C4 Co1 C6 . . 90.0(2) yes
C5 Co1 C6 . . 176.8(2) yes
Co1 C1 N1 . . 176.9(3) yes
Co1 C2 N2 . . 177.9(3) yes
Co1 C3 N3 . . 177.6(4) yes
Co1 C4 N4 . . 175.9(3) yes
Co1 C5 N5 . . 176.9(4) yes
Co1 C6 N6 . . 176.2(4) yes
K1 N7 C7 . . 86.5(2) no
K1 N7 C18 . . 157.3(2) no
C7 N7 C18 . . 113.4(3) no
C9 N8 C10 . . 117.0(3) no
C9 N8 K1 . 3_565 98.6(2) no
C10 N8 K1 . 3_565 112.2(2) no
C12 N9 C13 . . 117.2(3) no
C12 N9 K1 . 4_566 79.3(2) no
C13 N9 K1 . 4_566 145.7(2) no
C15 N10 C16 . . 117.7(3) no
C15 N10 K1 . 3_665 133.1(2) no
C16 N10 K1 . 3_665 97.8(2) no
N7 C7 C8 . . 114.7(3) no
C7 C8 C9 . . 112.0(3) no
N8 C9 C8 . . 113.1(3) no
N8 C10 C11 . . 112.5(3) no
C10 C11 C12 . . 107.2(3) no
N9 C12 C11 . . 113.8(3) no
N9 C13 C14 . . 111.7(3) no
C13 C14 C15 . . 111.0(3) no
N10 C15 C14 . . 110.9(3) no
N10 C16 C17 . . 113.2(3) no
C16 C17 C18 . . 109.5(3) no
N7 C18 C17 . . 112.4(3) 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
K1 N7 . 3.252(3) yes
K1 C7 . 3.497(4) yes
K1 N8 3_565 3.095(3) yes
K1 N9 4_565 3.352(3) yes
K1 N10 3_665 3.077(3) yes
Co1 C1 . 1.901(4) yes
Co1 C2 . 1.894(4) yes
Co1 C3 . 1.889(3) yes
Co1 C4 . 1.910(4) yes
Co1 C5 . 1.903(3) yes
Co1 C6 . 1.899(3) yes
C1 N1 . 1.142(5) yes
C2 N2 . 1.143(5) yes
C3 N3 . 1.151(5) yes
C4 N4 . 1.150(5) yes
C5 N5 . 1.140(5) yes
C6 N6 . 1.140(5) yes
N7 C7 . 1.502(5) yes
N7 C18 . 1.493(5) yes
N8 C9 . 1.503(5) yes
N8 C10 . 1.486(5) yes
N9 C12 . 1.508(5) yes
N9 C13 . 1.487(5) yes
N10 C15 . 1.490(5) yes
N10 C16 . 1.496(5) yes
C7 C8 . 1.520(5) no
C8 C9 . 1.510(5) no
C10 C11 . 1.529(5) no
C11 C12 . 1.518(6) no
C13 C14 . 1.527(5) no
C14 C15 . 1.516(5) no
C16 C17 . 1.529(6) no
C17 C18 . 1.502(5) no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
N1 N7 2.899(6) . no
N4 N8 2.909(6) 3_565 no
N6 N9 2.806(6) 2_555 no
N2 N10 2.916(6) 2_655 no
N5 N7 2.898(6) 3_665 no