#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003056.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_2003056 _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 'C14 H23 Co N10,2(H2 O)' _chemical_formula_sum 'C14 H27 Co N10 O2' _chemical_formula_iupac 'H3[Co(C N)6](C8 H20 N4),2(H2 O)' _chemical_formula_weight 426.37 _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 7.635(2) _cell_length_b 8.202(5) _cell_length_c 9.442(3) _cell_angle_alpha 109.080(10) _cell_angle_beta 103.460(10) _cell_angle_gamma 107.030(10) _cell_volume 497.7(4) _cell_formula_units_Z 1 _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 0.08 _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 224 _exptl_absorpt_coefficient_mu 0.894 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.851 _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w' _diffrn_reflns_number 2375 _diffrn_reflns_av_R_equivalents 0.1870 _diffrn_reflns_av_sigmaI/netI 0.0702 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -1.5 _reflns_number_total 2374 _reflns_number_observed 2015 _reflns_observed_criterion >4sigma(F) _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0802 _refine_ls_R_factor_obs 0.0614 _refine_ls_wR_factor_all 0.0820 _refine_ls_wR_factor_obs 0.0741 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.370 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_number_reflns 2015 _refine_ls_number_parameters 242 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment ; One H atom on O2W, and the acidic H atoms of the macrocycle can not be located from differential map ; _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo)+0.002(Fo^2^)]' _refine_ls_shift/esd_max 0.150 _refine_ls_shift/esd_mean 0.011 _refine_diff_density_max 0.850 _refine_diff_density_min -0.470 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.10(5) 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' '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 0.0000 0.0000 0.0000 0.0190(10) Uani d . 1 . Co C1 -0.1068(3) -0.2125(3) 0.0482(3) 0.0340(10) Uani d . 1 . C C2 0.2135(3) 0.1290(3) 0.2041(3) 0.0310(10) Uani d . 1 . C C3 0.0837(3) 0.2040(3) -0.0433(3) 0.0320(10) Uani d . 1 . C C4 -0.1921(3) -0.1299(3) -0.2050(3) 0.0290(10) Uani d . 1 . C C5 -0.1527(3) 0.1068(3) 0.0987(3) 0.0360(10) Uani d . 1 . C C6 0.1643(3) -0.1085(3) -0.0755(3) 0.0330(10) Uani d . 1 . C N1 -0.1506(3) -0.3420(3) 0.0647(3) 0.0660(10) Uani d . 1 . N N2 0.3225(3) 0.1964(3) 0.3223(3) 0.0570(10) Uani d . 1 . N N3 0.1400(3) 0.3316(3) -0.0799(3) 0.0710(10) Uani d . 1 . N N4 -0.3315(3) -0.2175(3) -0.3367(3) 0.0510(10) Uani d . 1 . N N5 -0.2505(3) 0.1810(3) 0.1454(3) 0.0980(10) Uani d . 1 . N N6 0.2563(3) -0.1745(3) -0.1367(3) 0.0900(10) Uani d . 1 . N N7 -0.2931(3) 0.2971(3) -0.1851(3) 0.0310(10) Uani d . 1 . N H7A -0.2061 0.2938 -0.1044 0.080 Uiso d R 1 . H N8 -0.6327(3) -0.0621(3) -0.4367(3) 0.0730(10) Uani d . 1 . N H8A -0.5160 -0.0714 -0.4098 0.080 Uiso d R 1 . H N9 -0.5935(3) -0.3615(3) -0.6614(3) 0.0330(10) Uani d . 1 . N N10 -0.3752(3) 0.0608(3) -0.5720(3) 0.0620(10) Uani d . 1 . N H10A -0.4926 0.0691 -0.5878 0.080 Uiso d R 1 . H C7 -0.4834(3) 0.2559(3) -0.2048(3) 0.0860(10) Uani d . 1 . C H7B -0.4999 0.3722 -0.1826 0.080 Uiso d R 1 . H H7C -0.4989 0.2224 -0.1187 0.080 Uiso d R 1 . H C8 -0.6565(3) 0.1117(3) -0.3447(3) 0.0460(10) Uani d . 1 . C H8B -0.7687 0.0758 -0.3147 0.080 Uiso d R 1 . H H8C -0.6848 0.1680 -0.4170 0.080 Uiso d R 1 . H C9 -0.7954(3) -0.2089(3) -0.5633(3) 0.0330(10) Uani d . 1 . C H9A -0.8389 -0.1623 -0.6397 0.080 Uiso d R 1 . H H9B -0.8971 -0.2389 -0.5208 0.080 Uiso d R 1 . H C10 -0.7823(3) -0.3874(3) -0.6521(3) 0.0730(10) Uani d . 1 . C H10B -0.8114 -0.4692 -0.6000 0.080 Uiso d R 1 . H H10C -0.8791 -0.4487 -0.7590 0.080 Uiso d R 1 . H C11 -0.5384(3) -0.2647(3) -0.7836(3) 0.0820(10) Uani d . 1 . C H11A -0.6410 -0.2302 -0.8274 0.080 Uiso d R 1 . H H11B -0.5182 -0.3487 -0.8703 0.080 Uiso d R 1 . H C12 -0.3536(3) -0.0938(3) -0.6700(3) 0.0530(10) Uani d . 1 . C H12A -0.2700 -0.1295 -0.6044 0.080 Uiso d R 1 . H H12B -0.2879 -0.0567 -0.7366 0.080 Uiso d R 1 . H C13 -0.1861(3) 0.2185(3) -0.4356(3) 0.0410(10) Uani d . 1 . C H13A -0.1024 0.2835 -0.4787 0.080 Uiso d R 1 . H H13B -0.1154 0.1645 -0.3801 0.080 Uiso d R 1 . H C14 -0.2347(3) 0.3568(3) -0.3220(3) 0.0910(10) Uani d . 1 . C H14A -0.1222 0.4749 -0.2690 0.080 Uiso d R 1 . H H14B -0.3409 0.3764 -0.3816 0.080 Uiso d R 1 . H O1W -0.3372(3) -0.5152(3) -0.7439(3) 0.0720(10) Uani d . 1 . O H1WA -0.2781 -0.4841 -0.6449 0.050 Uiso d R 1 . H H1WB -0.2639 -0.4716 -0.7896 0.050 Uiso d R 1 . H O2W 0.2737(3) -0.5132(3) -0.3581(3) 0.0990(10) Uani d . 1 . O H2WA 0.3354 -0.4539 -0.2570 0.050 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 0.0210(10) 0.0180(10) 0.0190(10) 0.0090(10) 0.0050(10) 0.0080(10) C1 0.0550(10) 0.0280(10) 0.0150(10) 0.0130(10) 0.0150(10) 0.0050(10) C2 0.0270(10) 0.0430(10) 0.0240(10) 0.0190(10) 0.0010(10) 0.0190(10) C3 0.0410(10) 0.0190(10) 0.0220(10) 0.0010(10) 0.0080(10) 0.0050(10) C4 0.0330(10) 0.0150(10) 0.0330(10) 0.0010(10) 0.0110(10) 0.0140(10) C5 0.0440(10) 0.0310(10) 0.0200(10) -0.0020(10) 0.0070(10) 0.0170(10) C6 0.0260(10) 0.0450(10) 0.0260(10) 0.0070(10) 0.0080(10) 0.0210(10) N1 0.1000(10) 0.0270(10) 0.0450(10) 0.0140(10) 0.0300(10) -0.0080(10) N2 0.0500(10) 0.0410(10) 0.0530(10) 0.0050(10) -0.0120(10) 0.0220(10) N3 0.1130(10) 0.0300(10) 0.0200(10) 0.0100(10) -0.0130(10) -0.0070(10) N4 0.0540(10) 0.0610(10) 0.0140(10) -0.0050(10) -0.0110(10) 0.0310(10) N5 0.0380(10) 0.0740(10) 0.1090(10) -0.0330(10) 0.0110(10) 0.0170(10) N6 0.0640(10) 0.1220(10) 0.0620(10) -0.0070(10) 0.0210(10) 0.0630(10) N7 0.0350(10) 0.0330(10) 0.0210(10) 0.0120(10) 0.0040(10) 0.0150(10) N8 0.0110(10) 0.0440(10) 0.1270(10) 0.0340(10) -0.0190(10) 0.0010(10) N9 0.0300(10) 0.0350(10) 0.0290(10) 0.0090(10) 0.0050(10) 0.0140(10) N10 0.610(10) 0.0080(10) 0.0710(10) -0.0050(10) -0.0320(10) 0.0190(10) C7 0.0560(10) 0.0440(10) 0.1110(10) 0.0370(10) -0.0350(10) 0.0030(10) C8 0.0460(10) 0.0480(10) 0.0260(10) 0.0030(10) 0.0130(10) 0.0100(10) C9 0.0420(10) 0.0260(10) 0.0300(10) 0.0100(10) 0.0150(10) 0.0120(10) C10 0.0120(10) 0.0060(10) 0.1350(10) -0.0130(10) -0.0190(10) 0.0040(10) C11 0.1060(10) 0.0220(10) 0.0660(10) 0.0130(10) -0.0420(10) 0.0200(10) C12 0.0510(10) 0.0520(10) 0.0310(10) 0.0020(10) 0.0250(10) -0.0030(10) C13 0.0100(10) 0.0540(10) 0.0390(10) 0.0160(10) -0.0010(10) -0.0020(10) C14 0.0920(10) 0.0220(10) 0.0990(10) -0.0020(10) 0.0040(10) -0.0010(10) O1W 0.0980(10) 0.0580(10) 0.1180(10) 0.0580(10) 0.0800(10) 0.0540(10) O2W 0.1100(10) 0.0650(10) 0.1540(10) 0.0460(10) 0.0920(10) 0.0460(10)