#------------------------------------------------------------------------------ #$Date: 2014-06-04 13:18:25 +0300 (Wed, 04 Jun 2014) $ #$Revision: 115562 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/51/65/1516507.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_1516507 loop_ _publ_author_name 'Duyker, Samuel G.' 'Halder, Gregory' 'Southon, Peter D.' 'Price, David J.' 'Edwards, Alison J.' 'Peterson, Vanessa K.' 'Kepert, Cameron' _publ_section_title ; Topotactic structural conversion and hydration-dependent thermal expansion in robust LnMIII(CN)6·nH2O and flexible ALnFeII(CN)6·nH2O frameworks (A = Li, Na, K; Ln = La-Lu, Y; M = Co, Fe; 0 ≤ n ≤ 5) ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/c4sc00809j _journal_year 2014 _chemical_formula_moiety 'C6 H10 Co1 La1 N6 O5' _chemical_formula_sum 'C6 H10 Co La N6 O5' _chemical_formula_weight 444.02 _chemical_name_common 'lanthanum(III) hexacyanidocobaltate(III) pentahydrate' _chemical_name_systematic 'lanthanum(III) hexacyanidocobaltate(III) pentahydrate' _space_group_IT_number 176 _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-P 6c' _symmetry_space_group_name_H-M 'P 63/m' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary geom _audit_creation_date 14-03-18 _audit_creation_method 'CRYSTALS_ver_14.30 + LaueG software' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 2 _cell_length_a 7.4597(11) _cell_length_b 7.4597(11) _cell_length_c 14.293(4) _cell_measurement_reflns_used 0 _cell_measurement_temperature 300 _cell_measurement_theta_max 0 _cell_measurement_theta_min 0 _cell_volume 688.8(2) _computing_cell_refinement 'LaueG (Piltz, 2011)' _computing_data_collection 'MAATEL/ANSTO control program' _computing_data_reduction 'argonne_boxes (Wilkinson et al., 1988) & LaueG (Piltz, 2011)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _diffrn_ambient_temperature 300 _diffrn_measured_fraction_theta_full 0.850 _diffrn_measured_fraction_theta_max 0.850 _diffrn_measurement_details '31 images, exposure time 100 minutes' _diffrn_radiation_wavelength 0.85 _diffrn_reflns_av_R_equivalents 0.1789 _diffrn_reflns_av_unetI/netI 0.0885 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 596 _diffrn_reflns_resolution_max 1.43 _diffrn_reflns_theta_full 70.44 _diffrn_reflns_theta_max 70.53 _diffrn_reflns_theta_min 0.443 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.0 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.141 _exptl_crystal_density_method 'not measured' _exptl_crystal_description ?block _exptl_crystal_F_000 192 _exptl_crystal_size_max 2 _exptl_crystal_size_mid 2 _exptl_crystal_size_min 2 _refine_diff_density_max 1.75 _refine_diff_density_min -2.64 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 0.9954 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 50 _refine_ls_number_reflns 558 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1199 _refine_ls_R_factor_gt 0.1180 _refine_ls_shift/su_max 0.0000176 _refine_ls_shift/su_mean 0.0000038 _refine_ls_structure_factor_coef F _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 3.73 1.42 2.70 1.13 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0935 _refine_ls_wR_factor_gt 0.0931 _refine_ls_wR_factor_ref 0.0927 _reflns_number_gt 574 _reflns_number_total 596 _reflns_threshold_expression >2sigma(I) _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _oxford_refine_ls_r_factor_ref 0.1153 _oxford_refine_ls_scale 0.714(8) _oxford_reflns_number_all 594 _oxford_reflns_threshold_expression_ref I>3.0\s(I) _[local]_cod_data_source_file c4sc00809j2.cif _[local]_cod_data_source_block LaCo(CN)6_5H2O_neutron _[local]_cod_cif_authors_sg_H-M 'P 63/m ' _[local]_cod_chemical_formula_sum_orig 'C6 H10 Co1 La1 N6 O5' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal' according to /usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius ; _cod_database_code 1516507 _iucr_refine_instruction_details_constraints ; FULL FIRST( X'S, U'S ) UNTIL LAST END ; _iucr_refine_instruction_details_restraints ; NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.02000 = O(2) TO H(2) U(IJ) .0, 0.02000 = O(2) TO H(2,5,1,1,1) U(IJ) .0, 0.02000 = O(2) TO H(2,3,1,1) U(IJ) .0, 0.02 = O(1) TO H(1) REM THERMSIM END (DO NOT REMOVE THIS LINE) END ; loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x-y,x,z+1/2 -x+y,-x,-z+1/2 -y,x-y,z y,-x+y,-z -x,-y,z+1/2 x,y,-z+1/2 -x+y,-x,z x-y,x,-z y,-x+y,z+1/2 -y,x-y,-z+1/2 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Co1 Co 0.0000 0.0000 0.0000 0.0098 1.0000 Uani S T C1 C 0.1339(3) -0.1022(3) 0.07565(15) 0.0206 1.0000 Uani . . O1 O 0.5717(11) 0.0593(7) 0.2500 0.0583 1.0000 Uani S TU N N 0.2153(3) -0.1667(3) 0.12136(15) 0.0396 1.0000 Uani . . La1 La 0.3333 -0.3333 0.2500 0.0106 1.0000 Uani S T O2 O 0.6667 0.3333 0.0844(6) 0.0612 1.0000 Uani S TU H1 H 0.621(2) 0.1296(14) 0.1934(12) 0.1301 1.0000 Uani . U H2 H 0.752(3) 0.337(4) 0.0388(13) 0.1056 0.6667 Uani . U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.010(2) 0.010(2) 0.010(4) 0.0000 0.0000 0.0049(11) C1 0.0240(8) 0.0240(9) 0.0173(8) 0.0020(6) -0.0058(6) 0.0145(7) O1 0.064(3) 0.0159(16) 0.077(4) 0.0000 0.0000 0.007(2) N 0.0447(10) 0.0441(11) 0.0398(10) 0.0091(7) -0.0133(7) 0.0295(8) La1 0.0108(7) 0.0108(7) 0.0100(12) 0.0000 0.0000 0.0054(4) O2 0.071(3) 0.071(3) 0.042(3) 0.0000 0.0000 0.0354(14) H1 0.144(9) 0.051(4) 0.139(10) 0.000(5) 0.074(8) 0.007(5) H2 0.110(10) 0.112(9) 0.097(9) 0.009(8) 0.021(8) 0.057(9) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 6.6484 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Co 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 2.4900 'International Tables Vol C 4.2.6.8 and 6.1.1.4' La 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 8.2400 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 9.3600 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 5.8050 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 -3.7409 'International Tables Vol C 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 10_555 Co1 C1 6_555 90.02(9) yes C1 10_555 Co1 C1 2_555 90.02(9) yes C1 6_555 Co1 C1 2_555 90.02(9) yes C1 10_555 Co1 C1 9_555 179.994 yes C1 6_555 Co1 C1 9_555 89.98(9) yes C1 2_555 Co1 C1 9_555 89.98(9) yes C1 10_555 Co1 C1 5_555 89.98(9) yes C1 6_555 Co1 C1 5_555 179.994 yes C1 2_555 Co1 C1 5_555 89.98(9) yes C1 9_555 Co1 C1 5_555 90.02(9) yes C1 10_555 Co1 C1 . 89.98(9) yes C1 6_555 Co1 C1 . 89.98(9) yes C1 2_555 Co1 C1 . 179.994 yes C1 9_555 Co1 C1 . 90.02(9) yes C1 5_555 Co1 C1 . 90.02(9) yes Co1 . C1 N0 . 179.21(19) yes H1 8_555 O1 La1 . 119.8(8) no H1 8_555 O1 H1 . 120.2(16) no La1 . O1 H1 . 119.8(8) no C1 . N0 La1 . 167.5(2) yes N0 12_545 La1 N0 8_555 75.74(8) yes N0 12_545 La1 N0 4_655 75.74(8) yes N0 8_555 La1 N0 4_655 75.74(8) yes N0 12_545 La1 N0 . 138.49(4) yes N0 8_555 La1 N0 . 89.72(10) yes N0 4_655 La1 N0 . 138.49(4) yes N0 12_545 La1 N0 9_655 138.49(4) yes N0 8_555 La1 N0 9_655 138.49(4) yes N0 4_655 La1 N0 9_655 89.72(10) yes N0 . La1 N0 9_655 75.74(8) yes N0 12_545 La1 N0 5_545 89.72(10) yes N0 8_555 La1 N0 5_545 138.49(4) yes N0 4_655 La1 N0 5_545 138.49(4) yes N0 . La1 N0 5_545 75.74(8) yes N0 9_655 La1 N0 5_545 75.74(8) yes N0 12_545 La1 O1 9_655 68.31(12) yes N0 8_555 La1 O1 9_655 135.12(5) yes N0 4_655 La1 O1 9_655 70.18(12) yes N0 . La1 O1 9_655 135.12(5) yes N0 9_655 La1 O1 9_655 70.18(12) yes N0 12_545 La1 O1 5_545 70.18(12) yes N0 8_555 La1 O1 5_545 68.31(12) yes N0 4_655 La1 O1 5_545 135.12(5) yes N0 . La1 O1 5_545 68.31(12) yes N0 9_655 La1 O1 5_545 135.12(5) yes N0 12_545 La1 O1 . 135.12(5) yes N0 8_555 La1 O1 . 70.18(12) yes N0 4_655 La1 O1 . 68.31(12) yes N0 . La1 O1 . 70.18(12) yes N0 9_655 La1 O1 . 68.31(12) yes N0 5_545 La1 O1 9_655 68.31(12) yes N0 5_545 La1 O1 5_545 70.18(12) yes O1 9_655 La1 O1 5_545 120.000(9) yes N0 5_545 La1 O1 . 135.12(5) yes O1 9_655 La1 O1 . 120.000(9) yes O1 5_545 La1 O1 . 120.000 yes H2 5_655 O2 H2 9_665 73.7(20) no H2 5_655 O2 H2 . 73.7(20) no H2 9_665 O2 H2 . 73.7(20) no 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 Co1 C1 10_555 1.8734(17) yes Co1 C1 6_555 1.8734(17) yes Co1 C1 2_555 1.8734(17) yes Co1 C1 9_555 1.8734(17) yes Co1 C1 5_555 1.8734(17) yes Co1 C1 . 1.8734(17) yes C1 N0 . 1.149(2) yes O1 H1 8_555 0.934(16) no O1 La1 . 2.556(5) yes O1 H1 . 0.934(16) no N0 La1 . 2.6065(17) yes O2 H2 5_655 0.90(2) no O2 H2 9_665 0.90(2) no O2 H2 . 0.90(2) no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag O1 H1 O2 159.1(12) 0.934 2.081 2.972(3) yes