#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003359.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_2003359 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 736 _journal_page_last 738 _publ_section_title ; 7,7-Dibromo-3-dibromomethylene-2,2-dimethyl-1-hydroxy-8,9,10-trinorbornane ; _chemical_formula_sum 'C10 H12 Br4 O' _chemical_formula_weight 467.84 _space_group_IT_number 4 _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _[local]_cod_cif_authors_sg_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.8937(6) _cell_length_b 7.7404(6) _cell_length_c 9.5873(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.528(9) _cell_angle_gamma 90.00 _cell_volume 659.76(8) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 2.355 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 20.28 _cell_measurement_theta_max 44.96 _exptl_absorpt_coefficient_mu 14.675 _cell_measurement_temperature 293(2) _exptl_crystal_description prism _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_colour colorless _chemical_compound_source ? _diffrn_measurement_device 'KM4 four-circle diffractometer' _diffrn_measurement_method \w/2\q _exptl_absorpt_correction_type 'DIFABS (Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 1.24 _diffrn_reflns_number 1461 _reflns_number_total 1385 _reflns_number_observed 1382 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_theta_max 75.09 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.5 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0329 _refine_ls_wR_factor_obs 0.0909 _refine_ls_wR_factor_all 0.0910 _refine_ls_goodness_of_fit_obs 1.094 _refine_ls_goodness_of_fit_all 1.094 _refine_ls_number_reflns 1385 _refine_ls_number_parameters 143 _refine_ls_hydrogen_treatment 'noref' _refine_ls_weighting_scheme ;calc w = 1/[\s^2^(Fo^2^) + (0.0561P)^2^ + 1.3243P] where P = (Fo^2^ + 2Fc^2^)/3 ; _refine_ls_shift/esd_max 0.001 _refine_diff_density_max 0.630 _refine_diff_density_min -0.596 _refine_ls_extinction_method 'SHELXL (Sheldrick, 1995)' _refine_ls_extinction_coef 0.0021(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0181 0.009 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0492 0.032 'Br' 'Br' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' -0.6763 1. _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack 0.05(6) loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv C1 1 0.6364(7) 0.3522(10) 0.1554(7) 0.0308(14) O1 1 0.4859(5) 0.3028(10) 0.1441(6) 0.0466(13) H1 1 0.4341(5) 0.3704(10) 0.1878(6) 0.166(86) C2 1 0.7005(7) 0.3373(11) 0.3097(7) 0.035(2) C21 1 0.6357(10) 0.1801(15) 0.3877(10) 0.054(2) H21A 1 0.6570(10) 0.0763(15) 0.3373(10) 0.066(20) H21B 1 0.5288(10) 0.1933(15) 0.3948(10) 0.066(20) H21C 1 0.6810(10) 0.1734(15) 0.4796(10) 0.066(20) C22 1 0.6624(10) 0.4988(19) 0.3962(11) 0.063(3) H22A 1 0.5563(10) 0.5016(19) 0.4118(11) 0.142(43) H22B 1 0.6911(10) 0.6007(19) 0.3464(11) 0.142(43) H22C 1 0.7162(10) 0.4945(19) 0.4843(11) 0.142(43) C3 1 0.8705(6) 0.3267(10) 0.2817(7) 0.0308(13) C31 1 0.9860(7) 0.3119(13) 0.3739(7) 0.040(2) Br31 1 0.96608(10) 0.3036(2) 0.56683(8) 0.0582(3) Br32 1 1.18650(7) 0.30281(14) 0.31561(9) 0.0502(3) C4 1 0.8892(7) 0.3438(9) 0.1258(7) 0.0308(14) H4 1 0.9861(7) 0.3052(9) 0.0907(7) 0.039(21) C5 1 0.8448(9) 0.5362(12) 0.0905(9) 0.047(2) H5A 1 0.8892(9) 0.6159(12) 0.1579(9) 0.028(13) H5B 1 0.8756(9) 0.5682(12) -0.0023(9) 0.028(13) C6 1 0.6726(8) 0.5325(11) 0.0996(9) 0.043(2) H6A 1 0.6380(8) 0.6212(11) 0.1625(9) 0.060(21) H6B 1 0.6253(8) 0.5503(11) 0.0084(9) 0.060(21) C7 1 0.7521(8) 0.2458(11) 0.0702(8) 0.038(2) Br71 1 0.72005(10) 0.2633(2) -0.13079(8) 0.0569(3) Br72 1 0.76657(10) -0.00079(12) 0.10599(10) 0.0507(3) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 C1 0.022(3) 0.000(2) 0.004(2) 0.034(4) 0.000(3) 0.037(3) O1 0.019(2) -0.006(3) 0.004(2) 0.062(4) -0.003(3) 0.059(3) C2 0.022(2) -0.003(3) 0.010(2) 0.043(5) 0.000(3) 0.040(3) C21 0.041(4) -0.018(4) 0.015(3) 0.071(7) 0.016(4) 0.049(5) C22 0.034(4) 0.021(5) -0.003(3) 0.095(8) -0.035(6) 0.058(5) C3 0.023(2) 0.002(3) 0.007(2) 0.027(4) 0.002(3) 0.042(3) C31 0.022(2) -0.006(4) 0.006(2) 0.052(5) 0.005(4) 0.046(3) Br31 0.0503(4) 0.0046(6) -0.0028(3) 0.0878(8) 0.0039(5) 0.0362(4) Br32 0.0223(3) 0.0018(4) 0.0003(3) 0.0706(6) 0.0110(5) 0.0576(4) C4 0.026(3) 0.003(3) 0.008(2) 0.030(4) 0.001(3) 0.036(3) C5 0.040(4) -0.008(3) 0.001(3) 0.040(5) 0.017(4) 0.059(5) C6 0.032(3) 0.001(3) 0.001(3) 0.035(5) 0.009(3) 0.062(5) C7 0.026(3) 0.003(3) 0.007(3) 0.041(5) 0.005(3) 0.046(4) Br71 0.0536(5) -0.0041(5) -0.0001(3) 0.0831(8) -0.0029(4) 0.0339(4) Br72 0.0490(5) 0.0018(4) 0.0000(4) 0.0348(5) -0.0056(4) 0.0682(5)