#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/00/2200048.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_2200048 loop_ _publ_author_name 'Aubauer, Christoph' 'Klap\"otke, Thomas M. ' 'Mayer, Peter' _publ_section_title ; 1,1,1,2,2-Pentaiododiphosphanium tetraiodogallate(III) ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first i1 _journal_page_last i2 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '(P2 I5) [Ga I4]' _chemical_formula_moiety 'P2 I5 1+, Ga I4 1-' _chemical_formula_sum 'Ga I9 P2' _chemical_formula_weight 1273.811 _chemical_name_common 'P2 I5 GaI4' _chemical_name_systematic ; 1,1,1,2,2-Pentaiododiphosphanium tetraiodogallate(III) ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _audit_creation_method 'form98_1/compatible with shelxl97-2' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 10.7960(5) _cell_length_b 18.1687(8) _cell_length_c 20.1886(10) _cell_measurement_reflns_used 5000 _cell_measurement_temperature 200(3) _cell_measurement_theta_max 24.0 _cell_measurement_theta_min 2.4 _cell_volume 3960.0(3) _computing_cell_refinement 'IPDS Software Manual' _computing_data_collection 'IPDS Software Manual (Stoe, 1997)' _computing_data_reduction 'IPDS Software Manual' _computing_molecular_graphics ; ORTEP-3 (Farrugia, 1997). SCHAKAL (Keller, 1995) and DIAMOND (Bergerhoff, 1996) ; _computing_publication_material 'PLATON (Spek, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR97 (Cascarano et al., 1996)' _diffrn_ambient_temperature 200(3) _diffrn_measured_fraction_theta_full .993 _diffrn_measured_fraction_theta_max .993 _diffrn_measurement_device 'image-plate area-detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'area detection' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0966 _diffrn_reflns_av_sigmaI/netI .0583 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 10907 _diffrn_reflns_theta_full 24.00 _diffrn_reflns_theta_max 24.00 _diffrn_reflns_theta_min 2.42 _exptl_absorpt_coefficient_mu 15.554 _exptl_absorpt_correction_T_max .395 _exptl_absorpt_correction_T_min .194 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; crystal faces optimized with Stoe XSHAPE (Stoe, 1997) then a numerical absorption correction with XRED (revision 1.09; Stoe, 1997) ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 4.2732(3) _exptl_crystal_density_method 'not measured' _exptl_crystal_description irregular _exptl_crystal_F_000 4304 _exptl_crystal_size_max .19 _exptl_crystal_size_mid .12 _exptl_crystal_size_min .10 _refine_diff_density_max '1.384 (0.82 \%A from I3)' _refine_diff_density_min '-1.230 (0.90 \%A from I3)' _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref .963 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 109 _refine_ls_number_reflns 3094 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all .963 _refine_ls_R_factor_all .036 _refine_ls_R_factor_gt .027 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0350P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .076 _reflns_number_gt 2570 _reflns_number_total 3094 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file na6005.cif _[local]_cod_data_source_block I _cod_database_code 2200048 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 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 Ga .13672(8) .21858(5) .11901(4) .0215(2) Uani d . 1 . . Ga I6 -.00354(5) .20184(3) .21770(3) .03203(16) Uani d . 1 . . I I7 .29375(5) .11255(3) .10729(3) .02884(16) Uani d . 1 . . I I8 .01101(6) .22888(3) .01348(3) .03364(16) Uani d . 1 . . I I9 .26802(5) .33435(3) .13418(3) .02882(16) Uani d . 1 . . I P1 .8024(2) .49494(11) .12882(11) .0224(5) Uani d . 1 . . P P2 .6664(2) .42147(12) .07874(11) .0239(5) Uani d . 1 . . P I1 .75379(5) .53586(3) .23890(3) .03010(16) Uani d . 1 . . I I2 .99534(5) .42794(3) .13111(3) .03039(16) Uani d . 1 . . I I3 .82519(6) .60032(4) .05889(4) .0455(2) Uani d . 1 . . I I4 .65420(6) .33280(3) .16800(3) .03460(17) Uani d . 1 . . I I5 .48824(5) .50114(3) .09895(3) .03056(16) Uani d . 1 . . I 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 Ga .0243(5) .0210(4) .0193(5) .0012(4) .0003(4) .0014(4) I6 .0364(3) .0306(3) .0291(3) -.0061(3) .0121(3) -.0023(3) I7 .0291(3) .0288(3) .0286(3) .0093(2) .0024(2) .0051(3) I8 .0420(4) .0345(3) .0245(3) .0055(3) -.0107(3) .0008(3) I9 .0227(3) .0270(3) .0368(3) -.0035(2) .0042(3) -.0007(3) P1 .0243(11) .0216(11) .0213(11) -.0011(8) .0014(9) .0023(10) P2 .0293(11) .0270(11) .0154(10) -.0014(9) -.0003(9) -.0029(10) I1 .0358(3) .0307(3) .0238(3) .0023(2) -.0058(3) -.0072(3) I2 .0254(3) .0246(3) .0412(4) .0018(2) .0021(3) -.0007(3) I3 .0445(4) .0377(4) .0543(5) .0032(3) .0106(3) .0234(3) I4 .0455(4) .0274(3) .0309(3) -.0066(3) -.0070(3) .0077(3) I5 .0276(3) .0322(3) .0319(3) .0000(2) -.0019(2) .0023(3) 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 Ga I6 . 2.5210(10) yes Ga I8 . 2.5330(10) yes Ga I9 . 2.5549(10) yes Ga I7 . 2.5771(10) yes P1 P2 . 2.227(3) yes P1 I3 . 2.391(2) yes P1 I1 . 2.401(2) yes P1 I2 . 2.413(2) yes P2 I4 . 2.421(2) yes P2 I5 . 2.442(2) yes loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga .2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -.4742 1.8119 '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 _geom_angle_publ_flag I6 Ga I8 110.60(4) yes I6 Ga I9 109.75(4) yes I8 Ga I9 109.71(4) yes I6 Ga I7 112.18(4) yes I8 Ga I7 109.30(4) yes I9 Ga I7 105.15(4) yes P2 P1 I3 106.25(11) yes P2 P1 I1 117.50(11) yes I3 P1 I1 108.72(8) yes P2 P1 I2 105.98(10) yes I3 P1 I2 109.04(9) yes I1 P1 I2 109.09(9) yes P1 P2 I4 95.56(10) yes P1 P2 I5 95.05(10) yes I4 P2 I5 103.13(9) yes loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 _geom_contact_publ_flag I1 I7 3.4420(9) 4_655 yes I2 I9 3.4002(8) 1_655 yes I4 I6 3.7264(8) 6_656 yes I5 I7 3.6598(8) 7_665 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag I3 P1 P2 I4 -174.24(8) no I1 P1 P2 I4 -52.33(12) no I2 P1 P2 I4 69.85(10) no I3 P1 P2 I5 -70.48(10) no I1 P1 P2 I5 51.43(12) no I2 P1 P2 I5 173.61(8) no _cod_database_fobs_code 2200048 _journal_paper_doi 10.1107/S1600536800018419