#------------------------------------------------------------------------------ #$Date: 2016-03-22 10:06:16 +0000 (Tue, 22 Mar 2016) $ #$Revision: 178934 $ #$URL: svn://www.crystallography.net/cod/cif/4/11/63/4116371.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_4116371 loop_ _publ_author_name 'Philip E. Eaton' 'Kakumanu Pramod' 'Todd Emrick' 'Richard Gilardi' _publ_contact_author ; Richard Gilardi Laboratory for the Structure of Matter The Naval Research Laboratory, Code 6030 Washington, D. C. ; USA 20375-5341 ; _publ_contact_author_email gilardi@nrl.navy.mil _publ_contact_author_fax '202 767 6874' _publ_contact_author_phone '202 404 2135' _publ_section_title ; Building with Cubane-1,4-diyl. Synthesis of Aryl-Substituted Cubanes, p-[n]Cubyls, and Cubane-Separated Bis(arenes)1 ; _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 4111 _journal_page_last 4123 _journal_paper_doi 10.1021/ja983441f _journal_volume 121 _journal_year 1999 _chemical_formula_sum 'C16 H12 I2' _chemical_formula_weight 458.06 _chemical_name_systematic ; ? ; _space_group_IT_number 166 _symmetry_cell_setting rhombohedral _symmetry_space_group_name_Hall '-R 3 2"' _symmetry_space_group_name_H-M 'R -3 m :H' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 3 _cell_length_a 8.9775(3) _cell_length_b 8.9775(3) _cell_length_c 15.3644(10) _cell_measurement_reflns_used 32 _cell_measurement_temperature 294(2) _cell_measurement_theta_max 15.03 _cell_measurement_theta_min 7.04 _cell_volume 1072.40(9) _computing_cell_refinement 'Siemens XSCANS' _computing_data_collection 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 294(2) _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_number 804 _diffrn_reflns_theta_max 28.97 _diffrn_reflns_theta_min 2.94 _diffrn_standards_decay_% 18.27 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 4.378 _exptl_absorpt_correction_T_max 0.4360 _exptl_absorpt_correction_T_min 0.2418 _exptl_absorpt_correction_type integration _exptl_crystal_colour clear _exptl_crystal_density_diffrn 2.128 _exptl_crystal_description almost-cubic_chunk _exptl_crystal_F_000 642 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _refine_diff_density_max 1.239 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.112 _refine_ls_extinction_coef 0.0016(5) _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_all 1.166 _refine_ls_goodness_of_fit_obs 1.215 _refine_ls_matrix_type full _refine_ls_number_parameters 27 _refine_ls_number_reflns 373 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.166 _refine_ls_restrained_S_obs 1.215 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_obs 0.0265 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0655 _refine_ls_wR_factor_obs 0.0631 _reflns_number_observed 323 _reflns_number_total 373 _reflns_observed_criterion >2sigma(I) _cod_data_source_file ja983441f_2.cif _cod_data_source_block eat32 _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M 'R -3 m' _cod_database_code 4116371 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' 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 I1 0.0828(3) 0.0828(3) 0.0235(3) 0.000 0.000 0.0414(2) C1 0.0382(14) 0.0382(14) 0.024(2) 0.000 0.000 0.0191(7) C2 0.0500(11) 0.0376(13) 0.0292(12) -0.0062(10) -0.0031(5) 0.0188(7) C3 0.0283(12) 0.0444(11) 0.0277(11) -0.0009(4) -0.0019(9) 0.0141(6) C4 0.0336(12) 0.0336(12) 0.020(2) 0.000 0.000 0.0168(6) 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags I1 I 0.3333 0.6667 0.52810(2) 0.0630(3) Uani 1 d S C1 C 0.3333 0.6667 0.3893(3) 0.0336(9) Uani 1 d S C2 C 0.4156(2) 0.8313(4) 0.3313(2) 0.0403(6) Uani 1 d S H2 H 0.4726(32) 0.9452(64) 0.3535(27) 0.048 Uiso 1 d S C3 C 0.4972(3) 0.7486(2) 0.2727(2) 0.0352(5) Uani 1 d S H3 H 0.6083(55) 0.8042(28) 0.2554(26) 0.042 Uiso 1 d S C4 C 0.3333 0.6667 0.2143(3) 0.0291(8) Uani 1 d S 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' I I -0.4742 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_site_symmetry_1 _geom_angle_site_symmetry_3 C2 C1 C2 90.6(2) 2_665 . C2 C1 C2 90.6(2) 2_665 3_565 C2 C1 C2 90.6(2) . 3_565 C2 C1 I1 124.8(2) 2_665 . C2 C1 I1 124.8(2) . . C2 C1 I1 124.8(2) 3_565 . C1 C2 C3 89.5(2) . . C1 C2 C3 89.5(2) . 2_665 C3 C2 C3 89.8(2) . 2_665 C4 C3 C2 90.0(2) . . C4 C3 C2 90.0(2) . 3_565 C2 C3 C2 90.3(3) . 3_565 C4 C4 C3 125.1(2) 25_565 2_665 C4 C4 C3 125.2(2) 25_565 . C3 C4 C3 90.2(2) 2_665 . C4 C4 C3 125.2(2) 25_565 3_565 C3 C4 C3 90.2(2) 2_665 3_565 C3 C4 C3 90.2(2) . 3_565 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 I1 C1 2.133(5) . C1 C2 1.559(4) 2_665 C1 C2 1.559(4) . C1 C2 1.559(4) 3_565 C2 C3 1.563(3) . C2 C3 1.563(3) 2_665 C3 C4 1.558(3) . C3 C2 1.563(3) 3_565 C4 C4 1.463(8) 25_565 C4 C3 1.558(3) 2_665 C4 C3 1.558(3) 3_565