#------------------------------------------------------------------------------ #$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/72/2007217.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, Tianyan' 'Crisci, Gerardo' 'Lu, Jian' 'Jacobson, Allan 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_paper_doi 10.1107/S0108270197018003 _journal_volume 54 _journal_year 1998 _chemical_formula_moiety 'Co(H~2~O)~2~Ni(CN)~4~ , 4H~2~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 ? _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 .0362 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0620P)^2^+1.1555P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.1069 _refine_ls_wR_factor_obs .1028 _reflns_number_observed 1139 _reflns_number_total 1706 _reflns_observed_criterion >2sigma(I) _cod_data_source_file bs1042.cif _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_enum 1527 2010-12-29 10:47:43Z saulius 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 The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'none' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0620P)^2^+1.1555P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0620P)^2^+1.1555P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _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 .0398(3) .0209(3) .0144(3) .000 .0015(2) .000 Co2 .0355(3) .0215(3) .0149(3) -.00205(19) .0011(2) -.00033(19) C1 .0358(15) .0263(15) .0205(12) -.0015(13) .0010(11) .0019(12) N1 .0431(15) .0338(14) .0230(11) -.0036(12) -.0004(11) -.0065(11) C2 .0366(16) .0296(16) .0215(13) .0007(13) -.0005(12) -.0033(12) N2 .0501(15) .0322(14) .0239(12) -.0031(13) .0011(12) .0052(11) O1 .0383(12) .0376(12) .0318(11) .0002(10) .0024(9) -.0020(10) O2 .0473(14) .0553(17) .0461(15) -.0028(13) -.0058(11) .0098(13) O3 .065(3) .056(3) .048(2) .000 .006(2) .000 O4 .061(2) .052(2) .054(2) .000 -.002(2) .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_disorder_group _atom_site_type_symbol Ni1 .56652(5) .7500 -.00766(6) .02504(18) Uani d S 1 . Ni Co2 .5000 .5000 -.5000 .02395(19) Uani d S 1 . Co C1 .5711(3) .6551(2) -.1921(4) .0275(6) Uani d . 1 . C N1 .5651(2) .5968(2) -.3031(3) .0333(6) Uani d . 1 . N C2 .5443(3) .6566(2) .1734(4) .0292(6) Uani d . 1 . C N2 .4734(2) .3998(2) -.2854(3) .0354(6) Uani d . 1 . N O1 .34317(18) .56012(17) -.4402(3) .0359(5) Uani d . 1 . O O2 .1785(2) .4353(2) -.5423(4) .0496(7) Uani d . 1 . O O3 .7920(4) .7500 .0598(6) .0564(10) Uani d S 1 . O O4 .2526(4) .2500 -.4514(6) .0555(10) Uani d S 1 . O H1A .2892 .5161 -.4933 .050 Uiso d . 1 . H H3A .7827 .7500 .1942 .050 Uiso d S 1 . H H2A .1964 .3781 -.5096 .050 Uiso d . 1 . H H1B .3377 .5531 -.3149 .050 Uiso d . 1 . H H2B .1632 .4486 -.6697 .050 Uiso d . 1 . H H4A .2038 .3000 -.5174 .050 Uiso d . 1 . H H3B .8342 .7500 -.0340 .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