#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003028.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_2003028 _journal_name_full 'Acta Crystallographica, Section B' _journal_year 1998 _journal_volume B54 _journal_page_first 431 _journal_page_last 437 _chemical_name_systematic Tetrakis(p-ter-butylbenzyl)Zirconium _chemical_formula_sum 'C44 H60 Zr1' _chemical_formula_weight 680.14 _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 16.481(2) _cell_length_b 16.481(2) _cell_length_c 7.131(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1937.0(10) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18 _cell_measurement_theta_max 22 _cell_measurement_temperature 293(2) _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max .5 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .3 _exptl_crystal_density_diffrn 1.166 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu .311 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min .86 _exptl_absorpt_correction_T_max 1.000 _diffrn_ambient_temperature 293(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71069 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 1512 _diffrn_reflns_av_R_equivalents .0000 _diffrn_reflns_av_sigmaI/netI .0322 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.5 _reflns_number_total 1512 _reflns_number_observed 1160 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all .0561 _refine_ls_R_factor_obs .033 _refine_ls_wR_factor_all .0919 _refine_ls_wR_factor_obs .0822 _refine_ls_goodness_of_fit_all 1.017 _refine_ls_goodness_of_fit_obs 1.053 _refine_ls_restrained_S_all 1.020 _refine_ls_restrained_S_obs 1.053 _refine_ls_number_reflns 1511 _refine_ls_number_parameters 102 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.6589P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/esd_max .001 _refine_ls_shift/esd_mean .000 _refine_diff_density_max .368 _refine_diff_density_min -.545 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Zr' 'Zr' -2.9673 .5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _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_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol Zr1 .5000 .0000 .2500 .0467(2) Uani d S 1 . Zr C1 .5057(2) .1007(2) .0322(5) .0582(8) Uani d . 1 . C C2 .5917(2) .1143(2) .0777(5) .0492(7) Uani d . 1 . C C3 .6533(2) .0647(2) .0070(5) .0533(8) Uani d . 1 . C C4 .7331(2) .0725(2) .0645(5) .0513(7) Uani d . 1 . C C5 .7561(2) .1287(2) .2001(5) .0514(8) Uani d . 1 . C C6 .6952(2) .1793(2) .2664(9) .0555(9) Uani d . 1 . C C7 .6162(2) .1721(2) .2111(5) .0550(11) Uani d . 1 . C C8 .8424(2) .1353(2) .2753(9) .0612(12) Uani d . 1 . C C9 .9011(3) .0758(3) .1826(9) .102(2) Uani d . 1 . C C10 .8415(3) .1161(3) .4885(8) .0832(13) Uani d . 1 . C C11 .8751(2) .2215(2) .2498(12) .0775(10) Uani d . 1 . C H1 .4950 .0829 -.0930 .070 Uiso d . 1 . H H2 .4707 .1458 .0590 .070 Uiso d . 1 . H H3 .6393 .0229 -.0820 .065 Uiso d . 1 . H H4 .7746 .0397 .0077 .062 Uiso d . 1 . H H5 .7093 .2222 .3471 .069 Uiso d . 1 . H H6 .5763 .2066 .2673 .068 Uiso d . 1 . H H7 .8823 .0223 .1944 .123 Uiso d . 1 . H H8 .9060 .0892 .0517 .123 Uiso d . 1 . H H9 .9536 .0808 .2384 .123 Uiso d . 1 . H H10 .8088 .1542 .5538 .100 Uiso d . 1 . H H11 .8217 .0630 .5099 .100 Uiso d . 1 . H H12 .8960 .1195 .5372 .100 Uiso d . 1 . H H13 .9284 .2249 .3039 .091 Uiso d . 1 . H H14 .8763 .2359 .1245 .091 Uiso d . 1 . H H15 .8409 .2588 .3190 .091 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 Zr1 .0522(2) .0522(2) .0356(2) .000 .000 .000 C1 .052(2) .074(2) .049(2) -.005(2) .000(2) .013(2) C2 .053(2) .052(2) .042(2) -.0033(13) .0031(14) .0092(14) C3 .061(2) .056(2) .043(2) -.0094(15) .0087(15) -.0083(14) C4 .052(2) .049(2) .053(2) -.0008(13) .010(2) -.0103(15) C5 .053(2) .0464(15) .055(2) -.0069(12) .0044(13) -.0052(13) C6 .061(2) .0449(13) .061(2) -.0040(11) .009(2) -.013(2) C7 .058(2) .0488(14) .059(3) .0036(12) .013(2) -.0020(14) C8 .0514(15) .060(2) .073(4) -.0054(13) -.006(2) -.007(2) C9 .056(2) .118(4) .132(6) .007(2) -.009(3) -.041(4) C10 .083(3) .086(3) .080(3) -.007(2) -.016(3) .018(3) C11 .071(2) .080(2) .082(2) -.028(2) -.021(4) .015(4)