data_2003054
_journal_name_full     'Acta Crystallographica, Section B'
_journal_year     1999
_journal_volume     B55
_journal_page_first     389
_journal_page_last     395
; Steve C.F. Au-Yeung
;
_chemical_formula_moiety     'C18 H32 Co K N12,4(H2 O)'
_chemical_formula_sum     'C18 H40 Co K N12 O4'
_chemical_formula_iupac     'K H2[Co(C N)6](C12 H30 N6).4(H2 O)'
_chemical_formula_weight     586.65
_symmetry_cell_setting     Triclinic
_symmetry_space_group_name_H-M     'P -1'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, -y, -z'
_cell_length_a     10.125(3)
_cell_length_b     11.133(2)
_cell_length_c     15.014(2)
_cell_angle_alpha     73.780(10)
_cell_angle_beta     71.680(10)
_cell_angle_gamma     68.87(2)
_cell_volume     1472.0(6)
_cell_formula_units_Z     2
_cell_measurement_reflns_used     25
_cell_measurement_theta_min     5
_cell_measurement_theta_max     15
_cell_measurement_temperature     293(2)
_exptl_crystal_description     Plate
_exptl_crystal_colour     Colorless
_exptl_crystal_size_max     0.30
_exptl_crystal_size_mid     0.30
_exptl_crystal_size_min     0.10
_exptl_crystal_density_diffrn     1.324
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     ?
_exptl_crystal_F_000     620
_exptl_absorpt_coefficient_mu     0.769
_exptl_absorpt_correction_type     Empirical
_exptl_absorpt_correction_T_min     0.833
_exptl_absorpt_correction_T_max     0.946
_diffrn_ambient_temperature     293(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device     'Siemens P4'
_diffrn_measurement_method     '\w'
_diffrn_reflns_number     4910
_diffrn_reflns_av_R_equivalents     0.0340
_diffrn_reflns_av_sigmaI/netI     0.0851
_diffrn_reflns_theta_min     1.45
_diffrn_reflns_theta_max     24.00
_diffrn_reflns_limit_h_min     0
_diffrn_reflns_limit_h_max     11
_diffrn_reflns_limit_k_min     -11
_diffrn_reflns_limit_k_max     12
_diffrn_reflns_limit_l_min     -16
_diffrn_reflns_limit_l_max     17
_diffrn_standards_number     3
_diffrn_standards_interval_count     100
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     -1.25
_reflns_number_total     4617
_reflns_number_observed     3032
_reflns_observed_criterion     >4sigma(F)
_refine_ls_structure_factor_coef     F
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0964
_refine_ls_R_factor_obs     0.0592
_refine_ls_wR_factor_all     0.0745
_refine_ls_wR_factor_obs     0.0667
_refine_ls_goodness_of_fit_obs     1.38
_refine_ls_restrained_S_all     ?
_refine_ls_restrained_S_obs     ?
_refine_ls_number_reflns     3023
_refine_ls_number_parameters     325
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     ?
_refine_ls_weighting_scheme     'calc w=1/[\s^2^(Fo)+0.0005Fo^2^]'
_refine_ls_shift/esd_max     0.001
_refine_ls_shift/esd_mean     0.000
_refine_diff_density_max     0.360
_refine_diff_density_min     -0.620
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
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'
    'K' 'K' 0.2009 0.2494
                         '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_
    _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_disorder_group
    _atom_site_type_symbol
    Co1 0.26070(10)
                  0.27640(10)
                            0.28940(10)
                                      0.0250(10)
                                               Uani d . 1 . Co
    C1 0.1670(7) 0.1451(6) 0.3620(4) 0.035(3) Uani d . 1 . C
    N1 0.1076(6) 0.0702(5) 0.4054(4) 0.048(3) Uani d . 1 . N
    C2 0.3494(7) 0.4107(6) 0.2223(4) 0.038(3) Uani d . 1 . C
    N2 0.3998(7) 0.4926(6) 0.1854(4) 0.061(3) Uani d . 1 . N
    C3 0.0782(7) 0.4080(6) 0.3063(4) 0.036(3) Uani d . 1 . C
    N3 -0.0325(7) 0.4876(6) 0.3142(4) 0.054(3) Uani d . 1 . N
    C4 0.2940(7) 0.2896(6) 0.4040(5) 0.037(3) Uani d . 1 . C
    N4 0.3185(7) 0.2939(6) 0.4724(4) 0.054(3) Uani d . 1 . N
    C5 0.4467(7) 0.1490(6) 0.2665(4) 0.035(3) Uani d . 1 . C
    N5 0.5575(6) 0.0730(6) 0.2514(4) 0.050(3) Uani d . 1 . N
    C6 0.2325(7) 0.2547(6) 0.1756(5) 0.038(3) Uani d . 1 . C
    N6 0.2167(7) 0.2382(6) 0.1083(4) 0.061(3) Uani d . 1 . N
    K1 -0.0057(2) -0.0181(2) 0.12730(10)
                                       0.0560(10)
                                                Uani d . 1 . K
    N11 -0.2878(5) 0.1178(5) 0.0404(4) 0.039(2) Uani d . 1 . N
    H11M -0.1964 0.1003 0.0034 0.050 Uiso d R 1 . H
    H11N -0.2855 0.0906 0.1024 0.050 Uiso d R 0.5 . H
    N12 -0.1567(6) 0.3214(5) -0.0442(4) 0.045(3) Uani d . 1 . N
    H12M -0.1919 0.3493 -0.0969 0.050 Uiso d R 1 . H
    N13 0.1399(5) 0.1870(5) -0.0389(3) 0.036(2) Uani d . 1 . N
    H13M 0.1504 0.1848 0.0201 0.050 Uiso d R 1 . H
    H13N 0.0752 0.1494 -0.0491 0.050 Uiso d R 0.5 . H
    C11 -0.3514(7) 0.0193(6) 0.0349(5) 0.043(3) Uani d . 1 . C
    H11A -0.3322 0.0144 -0.0310 0.060 Uiso d R 1 . H
    H11B -0.4552 0.0487 0.0589 0.060 Uiso d R 1 . H
    C12 -0.3747(7) 0.2553(6) 0.0151(5) 0.047(3) Uani d . 1 . C
    H12A -0.4701 0.2709 0.0573 0.060 Uiso d R 1 . H
    H12B -0.3850 0.2713 -0.0490 0.060 Uiso d R 1 . H
    C13 -0.2992(8) 0.3453(7) 0.0214(5) 0.050(3) Uani d . 1 . C
    H13A -0.3567 0.4351 0.0073 0.060 Uiso d R 1 . H
    H13B -0.2857 0.3278 0.0848 0.060 Uiso d R 1 . H
    C14 -0.0642(7) 0.3888(6) -0.0356(5) 0.048(3) Uani d . 1 . C
    H14A -0.0682 0.3776 0.0309 0.060 Uiso d R 1 . H
    H14B -0.0962 0.4809 -0.0609 0.060 Uiso d R 1 . H
    C15 0.0901(8) 0.3273(6) -0.0866(5) 0.046(3) Uani d . 1 . C
    H15A 0.0925 0.3316 -0.1518 0.060 Uiso d R 1 . H
    H15B 0.1538 0.3732 -0.0859 0.060 Uiso d R 1 . H
    C16 0.2899(7) 0.1173(6) -0.0884(4) 0.041(3) Uani d . 1 . C
    H16A 0.3534 0.1688 -0.0984 0.060 Uiso d R 1 . H
    H16B 0.2868 0.1098 -0.1498 0.060 Uiso d R 1 . H
    N21 0.1576(6) -0.3043(5) 0.4705(4) 0.050(3) Uani d . 1 . N
    H21M 0.1216 -0.3646 0.5156 0.060 Uiso d R 1 . H
    N22 -0.0101(7) -0.1100(5) 0.3476(4) 0.049(3) Uani d . 1 . N
    H22M 0.0417 -0.0901 0.3773 0.060 Uiso d R 1 . H
    N23 -0.2200(6) 0.1586(5) 0.4304(4) 0.043(3) Uani d . 1 . N
    H23M -0.1322 0.1403 0.4422 0.050 Uiso d R 1 . H
    H23N -0.3041 0.1493 0.4709 0.050 Uiso d R 1 . H
    C21 0.2979(8) -0.3494(7) 0.4924(6) 0.057(4) Uani d . 1 . C
    H21A 0.3355 -0.4431 0.5000 0.080 Uiso d R 1 . H
    H21B 0.3640 -0.3122 0.4402 0.080 Uiso d R 1 . H
    C22 0.1608(9) -0.3290(7) 0.3774(5) 0.061(4) Uani d . 1 . C
    H22A 0.2365 -0.3001 0.3285 0.080 Uiso d R 1 . H
    H22B 0.1804 -0.4209 0.3806 0.080 Uiso d R 1 . H
    C23 0.0202(8) -0.2534(6) 0.3533(5) 0.054(4) Uani d . 1 . C
    H23A -0.0551 -0.2829 0.4022 0.080 Uiso d R 1 . H
    H23B 0.0186 -0.2674 0.2934 0.080 Uiso d R 1 . H
    C24 -0.1668(8) -0.0391(7) 0.3622(5) 0.050(4) Uani d . 1 . C
    H24A -0.2034 -0.0627 0.3199 0.080 Uiso d R 1 . H
    H24B -0.2166 -0.0667 0.4265 0.080 Uiso d R 1 . H
    C25 -0.2009(9) 0.1085(7) 0.3438(5) 0.052(4) Uani d . 1 . C
    H25A -0.2880 0.1499 0.3206 0.080 Uiso d R 1 . H
    H25B -0.1218 0.1320 0.2951 0.080 Uiso d R 1 . H
    C26 -0.2851(8) 0.3060(7) 0.4179(5) 0.055(4) Uani d . 1 . C
    H26A -0.3797 0.3314 0.4053 0.080 Uiso d R 1 . H
    H26B -0.2242 0.3473 0.3646 0.080 Uiso d R 1 . H
    O1W 0.5410(6) 0.0953(7) 0.5561(4) 0.109(4) Uani d . 1 . O
    H1WA 0.4748 0.1553 0.5318 0.100 Uiso d R 1 . H
    H1WB 0.5514 0.0486 0.5168 0.100 Uiso d R 1 . H
    O2W 0.5361(7) 0.6723(7) 0.2006(5) 0.115(5) Uani d . 1 . O
    H2WA 0.4972 0.6191 0.1956 0.120 Uiso d R 1 . H
    H2WB 0.4752 0.7100 0.2456 0.120 Uiso d R 1 . H
    O3W -0.3176(6) 0.6593(6) 0.3319(4) 0.097(4) Uani d . 1 . O
    H3WA -0.2313 0.6072 0.3261 0.100 Uiso d R 1 . H
    H3WB -0.3374 0.6901 0.3819 0.100 Uiso d R 1 . H
    O4W 0.3133(9) 0.9111(7) 0.2125(6) 0.142(6) Uani d . 1 . O
    H4WA 0.2233 0.9258 0.2404 0.150 Uiso d R 1 . H
    H4WB 0.3860 0.8558 0.2328 0.150 Uiso d R 1 . H
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 0.0260(10)
                 0.0260(10)
                          0.0230(10)
                                   -0.0040(10)
                                             -0.0050(10)
                                                       -0.0100(10)
    C1 0.028(4) 0.034(4) 0.041(4) -0.007(3) -0.014(3) -0.003(3)
    N1 0.045(4) 0.042(3) 0.062(4) 0.001(3) -0.013(3) -0.027(3)
    C2 0.045(4) 0.040(4) 0.030(4) -0.009(3) -0.003(3) -0.017(4)
    N2 0.072(5) 0.060(4) 0.046(4) -0.03(3) 0.003(3) -0.036(4)
    C3 0.038(4) 0.030(4) 0.043(4) -0.004(3) -0.009(3) -0.017(3)
    N3 0.045(4) 0.044(4) 0.067(4) -0.010(3) -0.016(3) -0.004(3)
    C4 0.036(4) 0.034(4) 0.040(4) -0.006(3) -0.005(3) -0.013(3)
    N4 0.061(4) 0.068(4) 0.036(4) -0.016(3) -0.013(3) -0.017(3)
    C5 0.042(4) 0.042(4) 0.024(3) -0.006(3) -0.010(3) -0.016(4)
    N5 0.035(4) 0.060(4) 0.048(4) -0.015(3) -0.016(3) 0.004(3)
    C6 0.040(4) 0.040(4) 0.036(4) -0.005(3) -0.014(3) -0.009(3)
    N6 0.086(5) 0.060(4) 0.051(4) -0.012(3) -0.033(4) -0.022(4)
    K1 0.0590(10)
                0.0690(10)
                         0.0400(10)
                                  -0.0070(10)
                                            -0.0080(10)
                                                      -0.0240(10)
    N11 0.031(3) 0.046(3) 0.039(3) -0.003(3) -0.010(2) -0.012(3)
    N12 0.046(4) 0.042(3) 0.045(3) -0.008(3) -0.012(3) -0.010(3)
    N13 0.040(3) 0.037(3) 0.038(3) -0.006(2) -0.011(3) -0.019(3)
    C11 0.029(4) 0.053(4) 0.046(4) -0.011(3) -0.007(3) -0.012(3)
    C12 0.032(4) 0.039(4) 0.060(5) -0.006(3) -0.008(3) -0.004(3)
    C13 0.053(5) 0.040(4) 0.046(4) -0.013(3) -0.003(4) -0.006(4)
    C14 0.053(5) 0.028(4) 0.066(5) -0.006(3) -0.019(4) -0.014(3)
    C15 0.058(5) 0.039(4) 0.044(4) 0.000(3) -0.011(4) -0.025(4)
    C16 0.036(4) 0.052(4) 0.039(4) -0.012(3) -0.001(3) -0.023(3)
    N21 0.055(4) 0.046(3) 0.055(4) -0.015(3) -0.010(3) -0.021(3)
    N22 0.065(4) 0.040(3) 0.058(4) -0.008(3) -0.029(3) -0.023(3)
    N23 0.036(3) 0.052(4) 0.047(3) -0.004(3) -0.017(3) -0.018(3)
    C21 0.048(5) 0.048(4) 0.077(6) -0.023(4) -0.009(4) -0.012(4)
    C22 0.077(6) 0.048(5) 0.063(5) -0.027(4) -0.005(4) -0.021(4)
    C23 0.073(6) 0.046(4) 0.053(5) -0.012(4) -0.022(4) -0.022(4)
    C24 0.072(5) 0.054(5) 0.039(4) -0.03(3) -0.021(4) -0.031(4)
    C25 0.076(5) 0.061(5) 0.036(4) -0.003(3) -0.025(4) -0.034(4)
    C26 0.053(5) 0.044(4) 0.066(5) 0.001(4) -0.020(4) -0.016(4)
    O1W 0.063(4) 0.129(6) 0.105(5) 0.050(4) -0.033(4) -0.036(4)
    O2W 0.116(6) 0.113(6) 0.141(6) 0.004(5) -0.033(5) -0.083(5)
    O3W 0.069(4) 0.114(5) 0.089(4) -0.046(4) -0.021(4) 0.016(4)
    O4W 0.153(8) 0.115(6) 0.164(8) -0.020(6) -0.063(6) -0.029(6)