#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/82/2008286.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_2008286 loop_ _publ_author_name 'Boese, Roland' 'Bl\"aser, Dieter' 'Latz, R\"udiger' 'B\"aumen, Anja' _publ_section_title ; 2,2,5,5-Tetramethylhex-3-yne at 281K ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first IUC9900016 _journal_volume 55 _journal_year 1999 _chemical_formula_iupac 'C10 H18' _chemical_formula_sum 'C10 H18' _chemical_formula_weight 138.24 _chemical_melting_point .299E-298 _chemical_name_systematic ; 2,2,5,5-tetramethyl-hex-3-yne ; _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 17.836(4) _cell_length_b 9.805(2) _cell_length_c 5.8130(10) _cell_measurement_reflns_used 50 _cell_measurement_temperature 103(2) _cell_measurement_theta_max 25 _cell_measurement_theta_min 20 _cell_volume 1016.6(4) _computing_cell_refinement P3-VMS _computing_data_collection 'P3-VMS (Siemens, 1991a)' _computing_data_reduction 'XDISK (Siemens, 1991b)' _computing_molecular_graphics SHELXL97 _computing_publication_material SHELXL97 _computing_structure_refinement SHELXL97 _computing_structure_solution 'SHELXL97 (Sheldrick, 1997)' _diffrn_ambient_temperature 103(2) _diffrn_measured_fraction_theta_full 0.564 _diffrn_measured_fraction_theta_max 0.564 _diffrn_measurement_device_type 'Nicolet R3m/V four-circle' _diffrn_measurement_method 'Wyckoff-scan mode' _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 0.035 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_number 4389 _diffrn_reflns_theta_full 39.90 _diffrn_reflns_theta_max 39.90 _diffrn_reflns_theta_min 2.28 _diffrn_standards_decay_% <3 _diffrn_standards_interval_count 100 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 0.050 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 0.903 _exptl_crystal_density_method 'not measured' _exptl_crystal_description cylindrical _exptl_crystal_F_000 312 _exptl_crystal_size_max 3 _exptl_crystal_size_rad 0.15 _refine_diff_density_max 0.388 _refine_diff_density_min -0.184 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 93 _refine_ls_number_reflns 2001 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.063 _refine_ls_R_factor_gt 0.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0801P)^2^+0.1442P] where P = Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.145 _reflns_number_gt 1688 _reflns_number_total 2001 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file qa0089.cif _[local]_cod_data_source_block buaz0r _cod_database_code 2008286 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_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 C1 0.95999(6) 0.7500 0.0415(2) 0.0225(2) Uani d S 1 . . C C2 0.89834(6) 0.7500 -0.0420(2) 0.0229(2) Uani d S 1 . . C C3 0.82262(6) 0.7500 -0.1448(2) 0.0235(2) Uani d S 1 . . C C4 0.82964(8) 0.7500 -0.4061(3) 0.0456(5) Uani d S 1 . . C H4A 0.8559(9) 0.6744(18) -0.463(3) 0.063(5) Uiso d . 1 . . H H4B 0.7798(13) 0.7500 -0.477(4) 0.054(6) Uiso d S 1 . . H C5 0.78013(5) 0.62283(10) -0.0645(2) 0.0339(2) Uani d . 1 . . C H5A 0.7748(8) 0.6240(14) 0.109(3) 0.046(4) Uiso d . 1 . . H H5B 0.7321(8) 0.6235(14) -0.135(3) 0.045(4) Uiso d . 1 . . H H5C 0.8054(9) 0.5404(16) -0.109(3) 0.055(4) Uiso d . 1 . . H C6 1.03529(6) 0.7500 0.1470(2) 0.0230(2) Uani d S 1 . . C C7 1.04359(6) 0.62258(10) 0.2978(2) 0.0337(2) Uani d . 1 . . C H7A 1.0057(9) 0.6237(17) 0.428(3) 0.053(4) Uiso d . 1 . . H H7B 1.0375(7) 0.5377(15) 0.209(3) 0.045(4) Uiso d . 1 . . H H7C 1.0940(9) 0.6193(16) 0.369(3) 0.057(4) Uiso d . 1 . . H C8 1.09456(8) 0.7500 -0.0420(3) 0.0472(5) Uani d S 1 . . C H8A 1.1428(13) 0.7500 0.027(4) 0.057(6) Uiso d S 1 . . H H8B 1.0908(9) 0.6730(17) -0.142(3) 0.056(4) Uiso d . 1 . . H 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 C1 0.0197(4) 0.0242(5) 0.0237(5) 0.000 -0.0003(4) 0.000 C2 0.0198(4) 0.0252(5) 0.0236(5) 0.000 -0.0003(4) 0.000 C3 0.0164(4) 0.0309(5) 0.0232(5) 0.000 -0.0013(4) 0.000 C4 0.0237(6) 0.0905(14) 0.0227(6) 0.000 -0.0025(5) 0.000 C5 0.0253(4) 0.0307(4) 0.0457(6) -0.0062(3) -0.0036(4) -0.0011(4) C6 0.0168(4) 0.0283(5) 0.0239(5) 0.000 -0.0020(4) 0.000 C7 0.0332(4) 0.0279(4) 0.0401(5) 0.0042(3) -0.0108(4) 0.0026(4) C8 0.0208(5) 0.0887(15) 0.0320(7) 0.000 0.0033(5) 0.000 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 C1 C2 . 1.2022(15) ? C1 C6 . 1.4763(16) ? C2 C3 . 1.4767(15) ? C3 C4 . 1.524(2) ? C3 C5 7_575 1.5318(12) ? C3 C5 . 1.5319(12) ? C4 H4A . 0.937(17) ? C4 H4B . 0.98(2) ? C5 H5A . 1.015(15) ? C5 H5B . 0.951(14) ? C5 H5C . 0.961(16) ? C6 C8 . 1.5242(19) ? C6 C7 7_575 1.5336(12) ? C6 C7 . 1.5336(12) ? C7 H7A . 1.015(16) ? C7 H7B . 0.984(15) ? C7 H7C . 0.990(17) ? C8 H8A . 0.95(2) ? C8 H8B . 0.954(17) ? 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' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 -1 -1 3 0 -2 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 C2 C1 C6 . . 179.32(12) C1 C2 C3 . . 179.98(11) C2 C3 C4 . . 109.14(10) C2 C3 C5 . 7_575 109.22(7) C4 C3 C5 . 7_575 110.13(7) C2 C3 C5 . . 109.22(7) C4 C3 C5 . . 110.13(7) C5 C3 C5 7_575 . 108.97(11) C3 C4 H4A . . 113.0(10) C3 C4 H4B . . 110.1(12) H4A C4 H4B . . 107.8(12) C3 C5 H5A . . 109.9(8) C3 C5 H5B . . 108.0(9) H5A C5 H5B . . 110.2(12) C3 C5 H5C . . 111.8(9) H5A C5 H5C . . 108.6(13) H5B C5 H5C . . 108.3(12) C1 C6 C8 . . 109.38(11) C1 C6 C7 . 7_575 108.97(6) C8 C6 C7 . 7_575 110.19(7) C1 C6 C7 . . 108.97(6) C8 C6 C7 . . 110.19(7) C7 C6 C7 7_575 . 109.11(11) C6 C7 H7A . . 110.7(9) C6 C7 H7B . . 112.3(9) H7A C7 H7B . . 109.0(13) C6 C7 H7C . . 110.6(9) H7A C7 H7C . . 107.1(13) H7B C7 H7C . . 106.9(12) C6 C8 H8A . . 108.9(13) C6 C8 H8B . . 112.9(10) H8A C8 H8B . . 108.7(12)