#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003258.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_2003258 loop_ _publ_author_name 'Adovasio, V.' 'Nardelli, M.' _publ_section_title ; Metal--Hydroxy Ribbons in Pb(OH)(NCS) ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 380 _journal_page_last 382 _journal_volume 51 _journal_year 1995 _chemical_formula_analytical 'C H N O Pb S' _chemical_formula_moiety 'Pb (O H) (N C S)' _chemical_formula_sum 'C H N O Pb S' _chemical_formula_weight 282.29 _chemical_name_systematic ; Lead hydroxy thiocyanate ; _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2c 2ab' _symmetry_space_group_name_H-M 'P b n m' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.250(7) _cell_length_b 8.564(5) _cell_length_c 4.157(2) _cell_measurement_reflns_used 29 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 17.76 _cell_measurement_theta_min 12.07 _cell_volume 400.5(4) _computing_cell_refinement 'LQPARM (Nardelli & Mangia, 1984)' _computing_data_collection 'local programs' _computing_data_reduction 'local programs' _computing_molecular_graphics ; ORTEP (Johnson, 1965); PLUTO (Motherwell & Clegg, 1976) ; _computing_publication_material ; PARST (Nardelli, 1983); PARSTCIF (Nardelli, 1991) ; _computing_structure_refinement 'SHELXL93 (Sheldrick, 1994)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Siemens-AED single crystal diffractometer' _diffrn_measurement_method '\q-2\q scan' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1636 _diffrn_reflns_reduction_process ; Standard Lorentz and polarization correction. ; _diffrn_reflns_theta_max 26.97 _diffrn_reflns_theta_min 3.62 _diffrn_standards_decay_% 'within statitistical fluctuation' _diffrn_standards_interval_count 50 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 42.44 _exptl_absorpt_correction_T_max 0.354 _exptl_absorpt_correction_T_min 0.341 _exptl_absorpt_correction_type cylinder _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 4.682 _exptl_crystal_description 'slender needles' _exptl_crystal_F_000 480 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _refine_diff_density_max 2.637 _refine_diff_density_min -2.660 _refine_ls_extinction_coef 0.0050(10) _refine_ls_extinction_method 'F~c~^*^ = kF~c~[1+0.001\cF~c~^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_goodness_of_fit_obs 1.171 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 35 _refine_ls_number_reflns 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0264 _refine_ls_shift/esd_max <0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^)+(0.0324P)^2^] where P = (F~o~^2^+2F~c~^2^)/3 ; _refine_ls_wR_factor_obs 0.0579 _reflns_number_observed 383 _reflns_number_total 497 _reflns_observed_criterion I>2\s(I) _[local]_cod_data_source_file ha1124.cif _[local]_cod_data_source_block a _cod_database_code 2003258 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 'x, y, -z-1/2' '-x-1/2, 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 Pb 0.0202(3) 0.0262(3) 0.0227(3) 0.0000 0.0000 -0.0044(2) S 0.0242(16) 0.0307(19) 0.035(2) 0.0000 0.0000 0.0005(15) O 0.018(4) 0.019(4) 0.031(5) 0.0000 0.0000 0.008(4) N 0.028(7) 0.037(8) 0.053(9) 0.0000 0.0000 0.000(6) C 0.022(7) 0.026(7) 0.024(7) 0.0000 0.0000 -0.001(6) 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_type_symbol Pb 0.10941(4) 0.12978(6) 0.25000 0.0230(2) aniso Pb S -0.2302(3) 0.5839(4) 0.25000 0.0301(11) aniso S O 0.0055(8) -0.1113(11) 0.2500 0.023(2) ani O N -0.0528(12) 0.3506(15) 0.2500 0.039(3) ani N C -0.1244(11) 0.4477(16) 0.2500 0.024(3) ani C H 0.056(13) -0.170(16) 0.2500 0.02(4) iso N loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pb 'Lead ' -3.3944 10.1111 'IntTabC, 4.2.6.8, 6.1.1.4' 'S ' 'Sulphur ' 0.1246 0.1234 'IntTabC, 4.2.6.8, 6.1.1.4' 'O ' 'Oxygen ' 0.0106 0.0060 'IntTabC, 4.2.6.8, 6.1.1.4' 'N ' 'Nitrogen ' 0.0061 0.0033 'IntTabC, 4.2.6.8, 6.1.1.4' 'C ' 'Carbon ' 0.0033 0.0016 'IntTabC, 4.2.6.8, 6.1.1.4' 'H ' 'Hydrogen ' 0.0000 0.0000 'IntTabC, 4.2.6.8, 6.1.1.4' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 5 1 4 -6 1 5 -1 2 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_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N Pb O . . . 106.5(4) yes N Pb O . . 5 71.4(2) yes O Pb O . . 5 71.6(2) yes O Pb O . . 5_556 71.6(2) no O Pb O 5 . 5_556 115.8(4) yes O Pb N 5_556 . . 71.4(2) no Pb O Pb . . 5 108.4(2) yes Pb O Pb . 5 5 108.4(2) yes Pb O Pb . . 5_556 108.4(2) no Pb O Pb 5 . 5_556 115.8(4) no Pb N C . . . 179.9(12) yes S C N . . . 178.5(13) yes 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 Pb O . 2.372(9) yes Pb O 5 2.453(5) yes Pb N . 2.629(13) yes Pb O 5_556 2.453(5) no S C . 1.667(14) yes C N . 1.16(2) yes O H . 0.76(14) yes O Pb 5 2.453(5) no O Pb 5_556 2.453(5) no