#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003055.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_2003055 _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 H30 Co K N10' _chemical_formula_sum 'C18 H30 Co K N10' _chemical_formula_iupac 'K H2[Co(C N)6](C12 H28 N4)' _chemical_formula_weight 484.55 _chemical_melting_point ? _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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' _cell_length_a 10.675(2) _cell_length_b 10.516(2) _cell_length_c 21.051(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.89(3) _cell_angle_gamma 90.00 _cell_volume 2361.9(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5 _cell_measurement_theta_max 15 _cell_measurement_temperature 293(2) _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.928 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.942 _exptl_absorpt_correction_T_max 1.000 _diffrn_ambient_temperature 293(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source ; Rigaku RU-200 rotating-anode generator powered at 50kV and 90mA ; _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC7R' _diffrn_measurement_method '\w' _diffrn_reflns_number 5713 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0998 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -1.72 _reflns_number_total 5425 _reflns_number_observed 3133 _reflns_observed_criterion >4sigma(F) _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_R_factor_all 0.1070 _refine_ls_R_factor_obs 0.0489 _refine_ls_wR_factor_all 0.0625 _refine_ls_wR_factor_obs 0.0582 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.62 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_number_reflns 3133 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo)+0.0002Fo^2^]' _refine_ls_shift/esd_max 0.082 _refine_ls_shift/esd_mean 0.004 _refine_diff_density_max 0.310 _refine_diff_density_min -0.690 _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' 'Co' 'Co' 0.3494 0.9721 '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' 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 K1 0.18830(10) 0.48270(10) -0.12280(10) 0.0500(10) Uani d . 1 . K Co1 0.27730(10) 0.79670(10) 0.11540(10) 0.0240(10) Uani d . 1 . Co C1 0.2340(3) 0.6309(3) 0.0861(2) 0.0340(10) Uani d . 1 . C N1 0.2133(3) 0.5307(3) 0.0676(2) 0.0540(10) Uani d . 1 . N C2 0.2784(3) 0.7396(3) 0.2007(2) 0.0300(10) Uani d . 1 . C N2 0.2797(3) 0.7090(3) 0.2528(2) 0.0430(10) Uani d . 1 . N C3 0.3258(3) 0.9590(3) 0.1457(2) 0.0310(10) Uani d . 1 . C N3 0.3537(3) 1.0568(3) 0.1662(2) 0.0500(10) Uani d . 1 . N C4 0.2689(3) 0.8551(3) 0.0294(2) 0.0320(10) Uani d . 1 . C N4 0.2573(3) 0.8862(3) -0.0228(2) 0.0430(10) Uani d . 1 . N C5 0.4495(3) 0.7521(3) 0.1106(2) 0.0320(10) Uani d . 1 . C N5 0.5526(3) 0.7239(3) 0.1106(2) 0.0500(10) Uani d . 1 . N C6 0.1073(3) 0.8442(3) 0.1248(2) 0.0310(10) Uani d . 1 . C N6 0.0073(3) 0.8767(3) 0.1333(2) 0.0390(10) Uani d . 1 . N N7 0.2863(3) 0.3083(3) -0.0036(2) 0.0310(10) Uani d . 1 . N H(7) 0.2496 0.3735 0.0163 0.050 Uiso d R 1 . H H(7N) 0.3238 0.3241 -0.0405 0.050 Uiso d PR 0.5 . H N8 -0.0723(3) 0.2521(3) 0.1003(2) 0.0390(10) Uani d . 1 . N H(8) -0.1264 0.1966 0.0818 0.050 Uiso d R 1 . H H(8N) -0.1253 0.3173 0.1060 0.050 Uiso d PR 0.5 . H N9 0.1996(3) 0.2945(3) 0.2989(2) 0.0370(10) Uani d . 1 . N H(9) 0.2369 0.2500 0.3308 0.050 Uiso d R 1 . H H(9N) 0.1315 0.3148 0.3208 0.050 Uiso d PR 0.5 . H N10 0.5733(3) 0.3938(3) 0.1733(2) 0.0390(10) Uani d . 1 . N H(10) 0.6145 0.4637 0.1608 0.050 Uiso d R 1 . H H(10N) 0.6226 0.3490 0.2006 0.050 Uiso d PR 0.5 . H C7 0.1846(3) 0.2164(3) -0.0234(2) 0.0350(10) Uani d . 1 . C H(7A) 0.2233 0.1414 -0.0399 0.100 Uiso d R 1 . H H(7B) 0.1345 0.2538 -0.0572 0.100 Uiso d R 1 . H C8 0.0981(3) 0.1784(3) 0.0293(2) 0.0340(10) Uani d . 1 . C H(8A) 0.1481 0.1482 0.0649 0.100 Uiso d R 1 . H H(8B) 0.0441 0.1105 0.0151 0.100 Uiso d R 1 . H C9 0.0189(3) 0.2885(3) 0.0505(2) 0.0370(10) Uani d . 1 . C H(9A) 0.0730 0.3539 0.0675 0.100 Uiso d R 1 . H H(9B) -0.0260 0.3226 0.0141 0.100 Uiso d R 1 . H C10 -0.0193(3) 0.1949(3) 0.1598(2) 0.0420(10) Uani d . 1 . C H(10A) 0.0311 0.1226 0.1496 0.100 Uiso d R 1 . H H(10B) -0.0862 0.1658 0.1855 0.100 Uiso d R 1 . H C11 0.0614(3) 0.2887(3) 0.1987(2) 0.0420(10) Uani d . 1 . C H(11A) 0.0097 0.3523 0.2174 0.100 Uiso d R 1 . H H(11B) 0.1201 0.3298 0.1718 0.100 Uiso d R 1 . H C12 0.1301(3) 0.2131(3) 0.2505(2) 0.0420(10) Uani d . 1 . C H(12A) 0.0705 0.1608 0.2715 0.100 Uiso d R 1 . H H(12B) 0.1889 0.1577 0.2308 0.100 Uiso d R 1 . H C13 0.2822(3) 0.3959(3) 0.2744(2) 0.0370(10) Uani d . 1 . C H(13A) 0.3186 0.4436 0.3092 0.100 Uiso d R 1 . H H(13B) 0.2326 0.4530 0.2484 0.100 Uiso d R 1 . H C14 0.3870(3) 0.3410(3) 0.2350(2) 0.0360(10) Uani d . 1 . C H(14A) 0.3513 0.2857 0.2030 0.100 Uiso d R 1 . H H(14B) 0.4427 0.2919 0.2620 0.100 Uiso d R 1 . H C15 0.4606(3) 0.4460(3) 0.2040(2) 0.0370(10) Uani d . 1 . C H(15A) 0.4078 0.4870 0.1724 0.100 Uiso d R 1 . H H(15B) 0.4850 0.5081 0.2354 0.100 Uiso d R 1 . H C16 0.5530(3) 0.2978(3) 0.1215(2) 0.0390(10) Uani d . 1 . C H(16A) 0.5089 0.2265 0.1385 0.100 Uiso d R 1 . H H(16B) 0.6326 0.2681 0.1076 0.100 Uiso d R 1 . H C17 0.4772(3) 0.3494(3) 0.0643(2) 0.0430(10) Uani d . 1 . C H(17A) 0.5310 0.3653 0.0295 0.100 Uiso d R 1 . H H(17B) 0.4385 0.4281 0.0760 0.100 Uiso d R 1 . H C18 0.3773(3) 0.2554(3) 0.0448(2) 0.0480(10) Uani d . 1 . C H(18A) 0.4167 0.1815 0.0276 0.100 Uiso d R 1 . H H(18B) 0.3330 0.2298 0.0817 0.100 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 K(1) 0.0500(10) 0.0390(10) 0.0610(10) 0.0030(10) 0.0080(10) 0.0010(10) Co(1) 0.0250(10) 0.0210(10) 0.0270(10) -0.0050(10) 0.0020(10) 0.0000(10) C(1) 0.0320(10) 0.0330(10) 0.0360(10) -0.0070(10) -0.0030(10) 0.0010(10) N(1) 0.0510(10) 0.0360(10) 0.0740(10) -0.0210(10) -0.0010(10) 0.0000(10) C(2) 0.0270(10) 0.0250(10) 0.0390(10) -0.0050(10) 0.0020(10) -0.0030(10) N(2) 0.0450(10) 0.0470(10) 0.0380(10) 0.0050(10) 0.0020(10) -0.0030(10) C(3) 0.0340(10) 0.0300(10) 0.0290(10) 0.0040(10) 0.0040(10) -0.0010(10) N(3) 0.0650(10) 0.0310(10) 0.0550(10) -0.0110(10) 0.0030(10) -0.0090(10) C(4) 0.0280(10) 0.0280(10) 0.0390(10) -0.0100(10) 0.0010(10) -0.0010(10) N(4) 0.0520(10) 0.0470(10) 0.0300(10) -0.0010(10) 0.0010(10) -0.0020(10) C(5) 0.0370(10) 0.0340(10) 0.0260(10) -0.0050(10) 0.0050(10) 0.0030(10) N(5) 0.0360(10) 0.0680(10) 0.0460(10) -0.0040(10) 0.0060(10) 0.0150(10) C(6) 0.0330(10) 0.0260(10) 0.0320(10) 0.0000(10) 0.0010(10) -0.0020(10) N(6) 0.0280(10) 0.0410(10) 0.0470(10) -0.0020(10) 0.0080(10) 0.0000(10) N(7) 0.0360(10) 0.0310(10) 0.0250(10) -0.0020(10) 0.0020(10) -0.0050(10) N(8) 0.0280(10) 0.0370(10) 0.0510(10) -0.0090(10) 0.0020(10) -0.0050(10) N(9) 0.0390(10) 0.0410(10) 0.0310(10) 0.0080(10) 0.0090(10) 0.0080(10) N(10) 0.0310(10) 0.0480(10) 0.0380(10) -0.0020(10) 0.0020(10) -0.0080(10) C(7) 0.0400(10) 0.0330(10) 0.0330(10) -0.0070(10) 0.0000(10) -0.0070(10) C(8) 0.0350(10) 0.0250(10) 0.0420(10) 0.0040(10) 0.0050(10) -0.0040(10) C(9) 0.0350(10) 0.0330(10) 0.0410(10) 0.0040(10) 0.0000(10) -0.0010(10) C(10) 0.0470(10) 0.0320(10) 0.0480(10) -0.0060(10) 0.0140(10) -0.0080(10) C(11) 0.0480(10) 0.0340(10) 0.0450(10) -0.0010(10) -0.0010(10) 0.0010(10) C(12) 0.0490(10) 0.0360(10) 0.0430(10) 0.0040(10) 0.0100(10) 0.0030(10) C(13) 0.0390(10) 0.0370(10) 0.0360(10) -0.0040(10) 0.0040(10) 0.0000(10) C(14) 0.0340(10) 0.0340(10) 0.0410(10) -0.0020(10) 0.0070(10) 0.0030(10) C(15) 0.0420(10) 0.0350(10) 0.0350(10) -0.0030(10) 0.0040(10) -0.0050(10) C(16) 0.0310(10) 0.0450(10) 0.0420(10) -0.0110(10) 0.0000(10) 0.0020(10) C(17) 0.0430(10) 0.0440(10) 0.0420(10) 0.0020(10) -0.0030(10) -0.0040(10) C(18) 0.0490(10) 0.0430(10) 0.0510(10) 0.0090(10) -0.0160(10) -0.0060(10)