#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2007217.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_2007217 loop_ _publ_author_name 'Niu, T.' 'Crisci, G.' 'Lu, J.' 'Jacobson, A. J.' _publ_section_title ; Diaquacobalt Tetracyanonickelate Tetrahydrate ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 565 _journal_page_last 567 _journal_volume 54 _journal_year 1998 _chemical_formula_moiety 'Co(H2 O)2 Ni(C N)4 , 4H2 O' _chemical_formula_sum 'C4 H12 Co N4 Ni O6' _chemical_formula_weight 329.82 _chemical_name_systematic ; Diaquacobalt Tetracyanonickelate Tetrahydrate ; _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 12.178(3) _cell_length_b 13.885(3) _cell_length_c 7.143(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 11.52 _cell_measurement_theta_min 5.94 _cell_volume 1207.8(6) _computing_cell_refinement 'CAD4 software' _computing_data_collection 'CAD4 software (Enraf-Nonius, 1989)' _computing_data_reduction 'RC85 (Baird, 1985)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1996)' _computing_publication_material SHELXL96 _computing_structure_refinement 'SHELXL96 (Sheldrick, 1996b)' _computing_structure_solution 'SHELXS96 (Sheldrick, 1996a)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w scan' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1706 _diffrn_reflns_theta_max 27.95 _diffrn_reflns_theta_min 2.93 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.950 _exptl_absorpt_correction_T_max 0.554 _exptl_absorpt_correction_T_min 0.524 _exptl_absorpt_correction_type ; Empirical via \y scans (Enraf-Nonius, 1989) ; _exptl_crystal_colour Orange _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_meas none _exptl_crystal_density_method none _exptl_crystal_description Prism _exptl_crystal_F_000 668 _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.500 _refine_diff_density_min -0.501 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.061 _refine_ls_goodness_of_fit_obs 1.124 _refine_ls_hydrogen_treatment ; All H-atom parameters fixed ; _refine_ls_matrix_type full _refine_ls_number_parameters 79 _refine_ls_number_reflns 1366 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.061 _refine_ls_restrained_S_obs 1.124 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_obs 0.0362 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0620P)^2^+1.1555P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.1069 _refine_ls_wR_factor_obs 0.1028 _reflns_number_observed 1139 _reflns_number_total 1706 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file bs1042.cif _[local]_cod_data_source_block coni2 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' 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 2007217 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, 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 Ni1 0.0398(3) 0.0209(3) 0.0144(3) 0.000 0.0015(2) 0.000 Co2 0.0355(3) 0.0215(3) 0.0149(3) -0.00205(19) 0.0011(2) -0.00033(19) C1 0.0358(15) 0.0263(15) 0.0205(12) -0.0015(13) 0.0010(11) 0.0019(12) N1 0.0431(15) 0.0338(14) 0.0230(11) -0.0036(12) -0.0004(11) -0.0065(11) C2 0.0366(16) 0.0296(16) 0.0215(13) 0.0007(13) -0.0005(12) -0.0033(12) N2 0.0501(15) 0.0322(14) 0.0239(12) -0.0031(13) 0.0011(12) 0.0052(11) O1 0.0383(12) 0.0376(12) 0.0318(11) 0.0002(10) 0.0024(9) -0.0020(10) O2 0.0473(14) 0.0553(17) 0.0461(15) -0.0028(13) -0.0058(11) 0.0098(13) O3 0.065(3) 0.056(3) 0.048(2) 0.000 0.006(2) 0.000 O4 0.061(2) 0.052(2) 0.054(2) 0.000 -0.002(2) 0.000 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 Ni1 0.56652(5) 0.7500 -0.00766(6) 0.02504(18) Uani d S 1 Ni Co2 0.5000 0.5000 -0.5000 0.02395(19) Uani d S 1 Co C1 0.5711(3) 0.6551(2) -0.1921(4) 0.0275(6) Uani d . 1 C N1 0.5651(2) 0.5968(2) -0.3031(3) 0.0333(6) Uani d . 1 N C2 0.5443(3) 0.6566(2) 0.1734(4) 0.0292(6) Uani d . 1 C N2 0.4734(2) 0.3998(2) -0.2854(3) 0.0354(6) Uani d . 1 N O1 0.34317(18) 0.56012(17) -0.4402(3) 0.0359(5) Uani d . 1 O O2 0.1785(2) 0.4353(2) -0.5423(4) 0.0496(7) Uani d . 1 O O3 0.7920(4) 0.7500 0.0598(6) 0.0564(10) Uani d S 1 O O4 0.2526(4) 0.2500 -0.4514(6) 0.0555(10) Uani d S 1 O H1A 0.2892 0.5161 -0.4933 0.050 Uiso d . 1 H H3A 0.7827 0.7500 0.1942 0.050 Uiso d S 1 H H2A 0.1964 0.3781 -0.5096 0.050 Uiso d . 1 H H1B 0.3377 0.5531 -0.3149 0.050 Uiso d . 1 H H2B 0.1632 0.4486 -0.6697 0.050 Uiso d . 1 H H4A 0.2038 0.3000 -0.5174 0.050 Uiso d . 1 H H3B 0.8342 0.7500 -0.0340 0.050 Uiso d S 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 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' Ni Ni 0.3393 1.1124 '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' O O 0.0106 0.0060 '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' 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 C2 Ni1 C2 8_575 . 88.9(2) yes C2 Ni1 C1 . . 90.20(10) yes C1 Ni1 C1 . 8_575 90.0(2) yes N2 Co2 N2 5_664 . 180.00(10) yes N2 Co2 N1 . . 89.60(10) yes N1 Co2 N1 5_664 . 180.0 yes N2 Co2 O1 . . 88.60(10) yes N1 Co2 O1 . . 87.30(10) yes O1 Co2 O1 . 5_664 180.0 yes N1 C1 Ni1 . . 174.6(3) yes C1 N1 Co2 . . 161.4(3) yes N2 C2 Ni1 5_665 . 177.4(3) yes C2 N2 Co2 5_665 . 177.1(3) yes Co2 O1 O2 . . 110.70(10) yes Co2 O1 O3 . 6 120.10(10) yes Co2 O1 O2 . 2_565 107.00(10) yes O2 O1 O3 . 6 110.20(10) ? O2 O1 O2 . 2_565 102.20(10) ? O3 O1 O2 6 2_565 105.00(10) ? O1 O2 O4 . . 106.40(10) ? 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 Ni1 C2 . 1.851(3) yes Ni1 C1 . 1.864(3) yes Co2 N2 . 2.095(3) yes Co2 N1 . 2.101(3) yes Co2 O1 . 2.128(2) yes C1 N1 . 1.136(4) yes N2 C2 5_665 1.140(4) yes Ni1 O3 . 2.788(4) yes