#------------------------------------------------------------------------------ #$Date: 2009-12-10 18:47:15 +0200 (Thu, 10 Dec 2009) $ #$Revision: 936 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100912.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_1100912 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2000 _journal_volume 56 _journal_page_first 1289 _journal_page_last 1291 _publ_section_title ; Na~2~Fe(CN)~5~NO.2D~2~O at 11 and 293 K by X-ray and at 15 K by neutron diffraction ; loop_ _publ_author_name 'Schultz, Arthur J.' 'Figgis, Brian N.' 'Sobolev, Alexandre N.' _publ_section_synopsis ; Precise X-ray and neutron structural determinations of Na~2~Fe(CN)~5~NO.2D~2~O performed at very low temperatures are presented. The X-ray and neutron diffraction positional and atomic displacement parameters agree very well. The [Fe(CN)~5~NO]^2-^ anion has approximate octahedral stereochemistry. ; _chemical_name_systematic ; disodium pentacyanonitrosylferrate(III) bis(dideuterium oxide) ; _chemical_name_common 'Sodium nitroprusside, deuterated' _chemical_formula_moiety 'Na2 Fe (C N)5 N O , 2D2 O' _chemical_formula_sum 'C5 D4 Fe N6 Na2 O3' _chemical_formula_weight 301.97 _chemical_melting_point 'not measured' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnnm _symmetry_space_group_name_Hall '-P 2 2n' _cell_length_a 6.124(2) _cell_length_b 11.837(5) _cell_length_c 15.547(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1127.0(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8 _cell_measurement_theta_min 34.5 _cell_measurement_theta_max 34.5 _cell_measurement_temperature 11.0(10) _exptl_crystal_description prism _exptl_crystal_colour 'dark red-brown' _exptl_crystal_size_max .38 _exptl_crystal_size_mid .32 _exptl_crystal_size_min .29 _exptl_crystal_density_diffrn 1.780 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 1.419 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_process_details '(XTAL3.4; Hall et al., 1995)' _exptl_absorpt_correction_T_min .641 _exptl_absorpt_correction_T_max .705 _diffrn_ambient_temperature 11(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator none _diffrn_measurement_device_type 'Huber 512 goniometer' _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 44955 _diffrn_reflns_av_R_equivalents .028 _diffrn_reflns_av_sigmaI/netI .013 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 50.13 _diffrn_reflns_theta_full 50.13 _diffrn_measured_fraction_theta_max .990 _diffrn_measured_fraction_theta_full .990 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _reflns_number_total 6020 _reflns_number_gt 5342 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all .025 _refine_ls_R_factor_gt .020 _refine_ls_wR_factor_ref .054 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_number_reflns 6020 _refine_ls_number_parameters 95 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment refall _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0230P)^2^+0.2957P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max .002 _refine_ls_shift/su_mean .000 _refine_diff_density_max .98 _refine_diff_density_min -1.07 _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_extinction_coef .0096(6) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' D H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na .0362 .0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe .3463 .8444 '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_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Fe1 0.500791(12) .280406(6) 0.5 .00324(2) Uani d S 1 . . Fe Na1 0.5 0 0.245992(17) .00649(4) Uani d S 1 . . Na Na2 0 0 0.378142(18) .00712(4) Uani d S 1 . . Na O1 0.88845(8) .40507(4) 0.5 .01010(6) Uani d S 1 . . O O2 0.17170(6) .12253(3) 0.26872(2) .00956(4) Uani d . 1 . . O N1 0.72761(7) .35799(4) 0.5 .00550(5) Uani d S 1 . . N N2 0.09861(9) .12392(4) 0.5 .00859(6) Uani d S 1 . . N N3 0.66704(6) .11951(3) 0.35800(2) .00868(4) Uani d . 1 . . N N4 0.25023(6) .40559(3) 0.35539(2) .00944(5) Uani d . 1 . . N C1 0.24954(9) .18302(4) 0.5 .00629(6) Uani d S 1 . . C C2 0.60734(6) .17961(3) 0.41208(2) .00631(4) Uani d . 1 . . C C3 0.34600(6) .36209(3) 0.41082(2) .00647(4) Uani d . 1 . . C D1 0.180(2) .1871(11) 0.2860(9) .028(3) Uiso d . 1 . . D D2 0.067(2) .1251(12) 0.2343(9) .033(3) Uiso d . 1 . . D 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 Fe1 .00376(2) .00314(2) .00281(2) -.00007(2) 0 0 Na1 .00717(9) .00675(8) .00556(8) -.00082(7) 0 0 Na2 .00758(9) .00724(8) .00653(8) .00047(7) 0 0 O1 .00714(14) .00948(14) .01369(16) -.00352(11) 0 0 O2 .01005(11) .00910(9) .00953(10) .00055(8) -.00120(8) .00060(8) N1 .00570(13) .00509(12) .00571(12) -.00035(10) 0 0 N2 .00811(15) .00843(14) .00923(14) -.00269(12) 0 0 N3 .00936(11) .00908(10) .00760(10) .00131(8) .00026(8) -.00294(8) N4 .00994(12) .01124(11) .00715(10) .00196(9) -.00136(8) .00239(8) C1 .00650(15) .00627(14) .00611(13) -.00100(11) 0 0 C2 .00701(11) .00636(10) .00556(9) .00050(8) .00009(8) -.00097(8) C3 .00723(11) .00682(10) .00537(10) .00080(8) -.00038(8) .00079(8)