#------------------------------------------------------------------------------ #$Date: 2009-11-18 14:56:34 +0000 (Wed, 18 Nov 2009) $ #$Revision: 858 $ #$URL: svn://www.crystallography.net/cod/cif/2/2002900.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_2002900 _journal_name_full 'Acta Crystallographica, Section B' _journal_volume 54 _journal_year 1998 _journal_page_first 600 _journal_page_last 612 loop_ _publ_author_name 'Ptasiewicz-B\;ak, H.' 'Olovsson, I.' 'McIntyre, G.J.' _chemical_formula_moiety 'Ni C4 N4 Na2, 3H2 O' _chemical_formula_sum 'C4 H6 N4 Na2 Ni O3' _[local]_cod_chemical_formula_sum_orig 'H6 Ni1 Na2 C4 N4 O3' _chemical_formula_iupac 'Na2Ni(CN)4.3(H2 O)' _chemical_formula_weight 262.81 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P - 1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' _cell_length_a 7.320(2) _cell_length_b 8.902(2) _cell_length_c 15.204(4) _cell_angle_alpha 89.333(6) _cell_angle_beta 87.336(7) _cell_angle_gamma 83.621(6) _cell_volume 983.0(10) _cell_formula_units_Z 4 _cell_measurement_reflns_used 454 _cell_measurement_theta_min 3 _cell_measurement_theta_max 33.2 _cell_measurement_temperature 30 _exptl_crystal_description ;trapezoidal prism ; _exptl_crystal_colour orange _exptl_crystal_size_max 3.75 _exptl_crystal_size_mid 2.80 _exptl_crystal_size_min 1.65 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_meas 'not measured' _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_type ;Gaussian (Coppens, Leiserowitz & Rabinovich, 1965) ; _exptl_absorpt_correction_T_min 0.7532 _exptl_absorpt_correction_T_max 0.8646 _diffrn_radiation_type 'neutron' _diffrn_radiation_wavelength 0.8417(2) _diffrn_measurement_device ;D9 four-circle ; _diffrn_measurement_method '\w-x\q' _diffrn_reflns_number 4946 _diffrn_reflns_av_R_equivalents 0.015 _diffrn_reflns_theta_max 33.2 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 1 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _reflns_number_total 4377 _reflns_number_observed 4377 _reflns_observed_criterion 'all reflections used' _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0493 _refine_ls_wR_factor_obs 0.0685 _refine_ls_goodness_of_fit_obs 2.191 _refine_ls_number_reflns 4377 _refine_ls_number_parameters 365 _refine_ls_hydrogen_treatment ;refined ; _refine_ls_weighting_scheme ;w = 1/[\s^2^(F~o~^2^) + k^2^F~o~^4^] ; _refine_ls_shift/esd_max 0.01 _refine_diff_density_max ? _refine_diff_density_min ? _refine_ls_extinction_method ;Gaussian type I isotropic (Becker & Coppens, 1974, 1975) ; _refine_ls_extinction_coef 'y=0.89' _atom_type_scat_source 'Sears (1986)' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Ni1 .24971(10) .51153(8) .48292(5) .0046(3) Ni2 .25408(10) -.01180(8) .01299(5) .0042(3) Na1 .1864(3) .0758(2) .68890(10) .0077(9) Na2 .2600(3) .4319(2) .80710(10) .0075(9) Na3 .0468(3) .2418(2) .24320(10) .0067(8) Na4 .5 .0 .5 .0074(9) Na5 .5 .5 .0 .0072(10) O1 .4643(2) .6088(2) .85580(10) .0082(6) O2 .0059(2) .5917(2) .88050(10) .0079(6) O3 .4431(2) -.1104(2) .64410(10) .0080(6) O4 -.0327(2) -.0792(2) .63100(10) .0085(6) O5 .0067(2) .2876(2) .75930(10) .0090(6) O6 .4385(2) .2231(2) .73600(10) .0083(6) C1 .2290(2) .31190(10) .51750(10) .0068(5) C2 .2609(2) .45680(10) .36430(10) .0065(5) C3 .2324(2) .56690(10) .60130(10) .0067(5) C4 .2775(2) .71060(10) .44960(10) .0070(5) C5 .2873(2) .18440(10) -.02360(10) .0069(5) C6 .3089(2) .03410(10) .12840(10) .0066(5) C7 .2225(2) -.21190(10) .04490(10) .0066(5) C8 .1973(2) -.05350(10) -.10180(10) .0064(5) N1 .22240(10) .18710(10) .54090(10) .0088(4) N2 .26300(10) .42640(10) .28950(10) .0087(4) N3 .21600(10) .60200(10) .67530(10) .0085(4) N4 .29730(10) .83440(10) .42780(10) .0093(4) N5 .30930(10) .30620(10) -.04860(10) .0087(3) N6 .34020(10) .06440(10) .20030(10) .0084(4) N7 .20400(10) -.33790(10) .06200(10) .0084(4) N8 .16100(10) -.08060(10) -.17370(10) .0090(4) H11 .5683(4) .6015(4) .8133(2) .0250(10) H12 .4097(5) .7114(3) .8518(2) .0300(10) H21 .0401(5) .6361(4) .9334(2) .0300(10) H22 -.0818(4) .5235(3) .9010(2) .0250(10) H31 .5296(4) -.1079(4) .6902(2) .0250(10) H32 .4018(5) -.2091(3) .6479(2) .0290(10) H41 -.1348(4) -.0079(3) .6155(2) .0260(10) H42 -.0003(6) -.1327(4) .5775(2) .035(2) H51 -.0744(5) .3604(4) .7284(2) .0310(10) H52 -.0611(5) .2698(4) .8134(2) .0310(10) H61 .5143(5) .2305(4) .6832(2) .0290(10) H62 .5115(5) .1507(4) .7718(2) .0290(10)