#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2016427.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_2016427 loop_ _publ_author_name 'Weigand, Jan J.' 'Decken, Andreas' 'Burford, Neil' _publ_section_title ; Hexaphenylhexaphosphinane benzene solvate ; _journal_coeditor_code GA3071 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first o64 _journal_page_last o66 _journal_volume 64 _journal_year 2008 _chemical_formula_iupac 'C36 H30 P6 , C6 H6' _chemical_formula_moiety 'C36 H30 P6 , C6 H6' _chemical_formula_sum 'C42 H36 P6' _chemical_formula_weight 726.53 _chemical_name_systematic ; hexaphenylhexaphosphinane benzene solvate ; _space_group_IT_number 148 _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-R 3' _symmetry_space_group_name_H-M 'R -3 :H' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 3 _cell_length_a 12.533(5) _cell_length_b 12.533(5) _cell_length_c 20.763(6) _cell_measurement_reflns_used 4176 _cell_measurement_temperature 173.0(10) _cell_measurement_theta_max 28.262 _cell_measurement_theta_min 2.711 _cell_volume 2824.4(18) _computing_cell_refinement 'SMART (Bruker, 1999)' _computing_data_collection 'SMART (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 2006)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2000)' _computing_publication_material 'SHELXTL (Sheldrick, 2000)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997a)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997a)' _diffrn_ambient_temperature 173.0(10) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Bruker SMART1000/P4' _diffrn_measurement_method '\f and \w' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 6465 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_min 2.12 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.315 _exptl_absorpt_correction_T_max 0.9543 _exptl_absorpt_correction_T_min 0.8712 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1997b)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_description parallelepiped _exptl_crystal_F_000 1134 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.479 _refine_diff_density_min -0.183 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 73 _refine_ls_number_reflns 1426 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.104 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0300 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0399P)^2^+2.4743P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.0880 _reflns_number_gt 1279 _reflns_number_total 1426 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ga3071.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'R -3' _cod_database_code 2016427 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 'x, y, z' 2 '-y, x-y, z' 3 '-x+y, -x, z' 4 'x+2/3, y+1/3, z+1/3' 5 '-y+2/3, x-y+1/3, z+1/3' 6 '-x+y+2/3, -x+1/3, z+1/3' 7 'x+1/3, y+2/3, z+2/3' 8 '-y+1/3, x-y+2/3, z+2/3' 9 '-x+y+1/3, -x+2/3, z+2/3' 10 '-x, -y, -z' 11 'y, -x+y, -z' 12 'x-y, x, -z' 13 '-x+2/3, -y+1/3, -z+1/3' 14 'y+2/3, -x+y+1/3, -z+1/3' 15 'x-y+2/3, x+1/3, -z+1/3' 16 '-x+1/3, -y+2/3, -z+2/3' 17 'y+1/3, -x+y+2/3, -z+2/3' 18 'x-y+1/3, x+2/3, -z+2/3' 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 P P1 0.03927(3) 0.17046(3) 0.526123(16) 0.02631(14) Uani d . 1 C C1 0.07438(12) 0.31045(12) 0.48036(7) 0.0299(3) Uani d . 1 C C2 0.11195(14) 0.41695(14) 0.51600(9) 0.0424(4) Uani d . 1 H H2 0.1163 0.4142 0.5616 0.051 Uiso calc R 1 C C3 0.14316(17) 0.52714(15) 0.48576(12) 0.0568(5) Uani d . 1 H H3 0.1693 0.5997 0.5106 0.068 Uiso calc R 1 C C4 0.13634(16) 0.53161(16) 0.41987(12) 0.0575(5) Uani d . 1 H H4 0.1575 0.6073 0.3992 0.069 Uiso calc R 1 C C5 0.09891(16) 0.42664(18) 0.38372(9) 0.0512(5) Uani d . 1 H H5 0.0944 0.4302 0.3382 0.061 Uiso calc R 1 C C6 0.06778(15) 0.31565(15) 0.41362(8) 0.0403(4) Uani d . 1 H H6 0.0420 0.2434 0.3885 0.048 Uiso calc R 1 C C7 0.71104(17) 0.45848(16) 0.33338(9) 0.0481(4) Uani d . 1 H H7 0.7416 0.5448 0.3335 0.058 Uiso calc R 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 P1 0.0278(2) 0.0277(2) 0.0236(2) 0.01396(14) -0.00032(11) -0.00097(12) C1 0.0248(6) 0.0272(6) 0.0376(7) 0.0130(5) 0.0009(5) 0.0021(5) C2 0.0366(8) 0.0318(8) 0.0556(10) 0.0146(6) -0.0014(7) -0.0048(7) C3 0.0464(10) 0.0284(8) 0.0901(16) 0.0147(7) -0.0014(9) -0.0004(8) C4 0.0372(9) 0.0362(9) 0.0977(17) 0.0172(7) 0.0087(9) 0.0261(9) C5 0.0417(9) 0.0557(11) 0.0568(11) 0.0249(8) 0.0071(8) 0.0257(8) C6 0.0418(8) 0.0399(8) 0.0400(8) 0.0210(7) 0.0019(6) 0.0071(6) C7 0.0538(10) 0.0429(9) 0.0463(10) 0.0233(8) -0.0008(7) 0.0003(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 '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' 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 _geom_angle_publ_flag C1 P1 P1 . 12_556 97.83(5) y C1 P1 P1 . 11_556 96.21(5) y P1 P1 P1 12_556 11_556 98.17(2) y C2 C1 C6 . . 119.06(14) y C2 C1 P1 . . 116.46(12) y C6 C1 P1 . . 124.47(11) y C3 C2 C1 . . 120.62(18) y C3 C2 H2 . . 119.7 ? C1 C2 H2 . . 119.7 ? C4 C3 C2 . . 120.02(18) y C4 C3 H3 . . 120.0 ? C2 C3 H3 . . 120.0 ? C3 C4 C5 . . 120.15(16) y C3 C4 H4 . . 119.9 ? C5 C4 H4 . . 119.9 ? C4 C5 C6 . . 120.26(18) y C4 C5 H5 . . 119.9 ? C6 C5 H5 . . 119.9 ? C5 C6 C1 . . 119.89(16) y C5 C6 H6 . . 120.1 ? C1 C6 H6 . . 120.1 ? C7 C7 C7 18_545 17 119.997(2) y C7 C7 H7 18_545 . 120.0 ? C7 C7 H7 17 . 120.0 ? 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 P1 C1 . 1.8446(15) y P1 P1 12_556 2.2207(8) y P1 P1 11_556 2.2207(8) y C1 C2 . 1.386(2) y C1 C6 . 1.392(2) y C2 C3 . 1.383(2) y C2 H2 . 0.9500 n C3 C4 . 1.374(3) y C3 H3 . 0.9500 n C4 C5 . 1.377(3) y C4 H4 . 0.9500 n C5 C6 . 1.389(2) y C5 H5 . 0.9500 n C6 H6 . 0.9500 n C7 C7 18_545 1.3774(18) y C7 C7 17 1.3774(18) y C7 H7 . 0.9500 n