#------------------------------------------------------------------------------ #$Date: 2011-09-28 16:24:46 +0200 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/04/2100430.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_2100430 _journal_coeditor_code DE5025 _journal_date_accepted 2006-01-08 _journal_date_recd_electronic 2005-11-02 _journal_issue 2 _journal_name_full 'Acta Crystallographica, Section B' _journal_page_first 321 _journal_page_last 329 _journal_paper_category FA _journal_volume 62 _journal_year 2006 _chemical_formula_sum 'Cl6 N3 P3' _chemical_formula_weight 347.64 _chemical_name_systematic ; Hexachlorocyclotriphosphazene ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 13.8572(8) _cell_length_b 12.8086(11) _cell_length_c 6.0801(5) _cell_measurement_reflns_used 1403 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 2.91 _cell_volume 1079.17(14) _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_molecular_graphics 'PLATON (Spek, 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 120(2) _diffrn_detector_area_resol_mean 9.091 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD Area Detector' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0185 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 7733 _diffrn_reflns_theta_full 27.49 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_min 2.94 _diffrn_standards_decay_% negligible _exptl_absorpt_coefficient_mu 1.986 _exptl_absorpt_correction_T_max 0.8262 _exptl_absorpt_correction_T_min 0.4368 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.140 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 672 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.671 _refine_diff_density_min -0.685 _refine_ls_extinction_coef 0.0213(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.261 _refine_ls_matrix_type full _refine_ls_number_parameters 62 _refine_ls_number_reflns 1283 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.261 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0275 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+0.3798P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.0735 _reflns_number_gt 1194 _reflns_number_total 1283 _reflns_threshold_expression >2sigma(I) _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 ; _cod_database_code 2100430 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' loop_ _atom_site_type_symbol _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 N N1 0.64922(15) 0.7500 0.5951(4) 0.0187(5) Uani d S 1 N N2 0.49315(11) 0.64417(11) 0.4448(2) 0.0181(3) Uani d . 1 P P1 0.59531(3) 0.64294(3) 0.55879(7) 0.01317(16) Uani d . 1 P P2 0.43947(4) 0.7500 0.39325(10) 0.01308(18) Uani d S 1 Cl Cl1 0.58539(3) 0.57022(4) 0.84708(7) 0.02287(16) Uani d . 1 Cl Cl2 0.68240(3) 0.54925(4) 0.39215(8) 0.02194(16) Uani d . 1 Cl Cl3 0.31285(4) 0.7500 0.54745(11) 0.02096(18) Uani d S 1 Cl Cl4 0.39841(5) 0.7500 0.08080(10) 0.02267(19) Uani d S 1 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 N1 0.0111(9) 0.0146(10) 0.0305(12) 0.000 -0.0067(9) 0.000 N2 0.0126(7) 0.0139(7) 0.0278(8) -0.0005(5) -0.0068(6) -0.0011(6) P1 0.0108(3) 0.0123(3) 0.0163(3) 0.00129(15) -0.00187(15) 0.00004(16) P2 0.0099(3) 0.0142(3) 0.0152(3) 0.000 -0.0025(2) 0.000 Cl1 0.0268(3) 0.0243(3) 0.0175(2) 0.00142(18) 0.00102(17) 0.00455(17) Cl2 0.0205(2) 0.0217(3) 0.0236(3) 0.00652(17) 0.00390(17) -0.00308(17) Cl3 0.0138(3) 0.0267(4) 0.0223(3) 0.000 0.0039(2) 0.000 Cl4 0.0212(3) 0.0320(4) 0.0147(3) 0.000 -0.0039(2) 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 P1 N1 P1 . 7_575 120.80(13) P1 N2 P2 . . 121.29(9) N2 P1 N1 . . 118.57(9) N2 P1 Cl2 . . 109.17(6) N1 P1 Cl2 . . 108.05(8) N2 P1 Cl1 . . 109.26(6) N1 P1 Cl1 . . 108.45(9) Cl2 P1 Cl1 . . 102.07(3) N2 P2 N2 7_575 . 118.46(11) N2 P2 Cl4 7_575 . 109.01(6) N2 P2 Cl4 . . 109.01(6) N2 P2 Cl3 7_575 . 108.79(6) N2 P2 Cl3 . . 108.79(6) Cl4 P2 Cl3 . . 101.44(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance N1 P1 . 1.5771(11) N1 P1 7_575 1.5771(11) N2 P1 . 1.5763(15) N2 P2 . 1.5777(15) P1 Cl2 . 1.9806(6) P1 Cl1 . 1.9897(6) P2 N2 7_575 1.5777(15) P2 Cl4 . 1.9831(9) P2 Cl3 . 1.9894(9)