#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/30/2003029.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_2003029 loop_ _publ_author_name 'Tedesco, C.' 'Immirzi, A.' 'Proto, A.' _publ_section_title ; Structures of Homoleptic Benzyl Derviatives of Zirconium ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 431 _journal_page_last 437 _journal_volume 54 _journal_year 1998 _chemical_formula_structural Zr(CH_2C_6H_5)_4 _chemical_formula_sum 'C28 H28 Zr' _chemical_formula_weight 455.72 _chemical_name_common Tetrakis(benzyl)Zirconium _chemical_name_systematic ; ? ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 16.3870(10) _cell_length_b 20.0220(10) _cell_length_c 13.758(6) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 22 _cell_measurement_theta_min 18 _cell_volume 4514(2) _computing_data_reduction 'TEXSAN (Molecular Structure Corp., 1992)' _computing_molecular_graphics 'TEXSAN (Molecular Structure Corp., 1992)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SIR92 (Altomare et al., 1992)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71069 _diffrn_reflns_av_R_equivalents .0000 _diffrn_reflns_av_sigmaI/netI .0599 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 6593 _diffrn_reflns_theta_max 30 _diffrn_reflns_theta_min 2.03 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu .498 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min .88 _exptl_absorpt_correction_type empirical _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.341 _exptl_crystal_description prism _exptl_crystal_F_000 1888 _exptl_crystal_size_max .8 _exptl_crystal_size_mid .7 _exptl_crystal_size_min .6 _refine_diff_density_max .463 _refine_diff_density_min -.454 _refine_ls_extinction_coef .0028(2) _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_all 1.001 _refine_ls_goodness_of_fit_obs 1.084 _refine_ls_matrix_type full _refine_ls_number_parameters 263 _refine_ls_number_reflns 6567 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.478 _refine_ls_restrained_S_obs 1.084 _refine_ls_R_factor_all .1634 _refine_ls_R_factor_obs .0362 _refine_ls_shift/esd_max -1.804 _refine_ls_shift/esd_mean .447 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+4.6197P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all .2267 _refine_ls_wR_factor_obs .0969 _reflns_number_observed 2347 _reflns_number_total 6593 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file na0084.cif _[local]_cod_data_source_block zrte _[local]_cod_cif_authors_sg_H-M Pbca _[local]_cod_chemical_formula_sum_orig 'C28 H28 Zr1' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 4514.(2) _cod_database_code 2003029 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 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 .0529(2) .0851(3) .0547(2) -.0013(2) .0052(2) .0060(2) C1A .072(3) .143(5) .062(3) .022(3) .014(2) .031(3) C2A .049(2) .113(4) .054(3) .006(3) .012(2) .006(3) C3A .068(3) .111(4) .051(2) .002(3) .012(2) .005(3) C4A .091(4) .095(4) .079(3) .001(3) .015(3) .016(3) C5A .085(4) .091(5) .155(6) -.009(4) .035(4) .007(5) C6A .067(4) .125(6) .152(7) -.027(4) .015(4) -.046(5) C7A .050(3) .162(6) .084(4) -.002(4) -.004(3) -.017(4) C1B .056(2) .101(4) .077(3) -.004(2) .010(2) -.017(3) C2B .051(2) .067(3) .067(3) .012(2) .002(2) -.013(2) C7B .072(3) .076(3) .069(3) .013(2) .003(2) .000(2) C6B .092(4) .083(4) .079(3) .014(3) -.013(3) -.005(3) C5B .066(3) .075(4) .113(5) .009(3) -.027(3) -.011(3) C4B .057(3) .092(4) .102(4) .008(2) .005(3) .001(3) C3B .062(3) .078(3) .068(3) .012(2) .005(2) -.004(2) C1C .091(4) .077(3) .077(3) .001(3) -.010(3) .002(3) C2C .068(3) .064(3) .064(2) .001(2) -.006(2) -.010(2) C7C .062(3) .080(3) .090(3) -.004(2) -.008(2) -.013(3) C6C .076(4) .105(4) .085(4) -.028(3) .000(3) -.003(3) C5C .104(5) .120(5) .096(4) -.038(4) -.023(4) .034(4) C4C .089(4) .072(3) .128(5) .002(3) -.021(4) .011(3) C3C .077(3) .057(3) .094(3) .006(2) .007(3) -.012(2) C1D .093(4) .125(5) .056(3) -.042(3) -.015(2) .017(3) C2D .075(3) .090(4) .035(2) -.012(3) -.005(2) -.003(2) C7D .119(5) .071(4) .066(3) -.010(3) -.011(3) .005(3) C6D .113(5) .094(5) .081(4) .028(4) .002(3) .003(3) C5D .067(4) .128(6) .101(4) .004(4) -.007(3) -.004(4) C4D .083(4) .087(4) .126(5) -.008(3) -.024(3) -.030(4) C3D .076(3) .069(3) .087(3) .003(3) -.014(3) -.026(3) 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 .26510(2) .15741(2) 1.50281(3) .0642(2) Uani d . 1 . Zr C1A .1422(3) .1858(3) 1.5647(3) .092(2) Uani d . 1 . C C2A .1364(3) .1184(3) 1.5997(3) .0719(13) Uani d . 1 . C C3A .1799(3) .0977(3) 1.6817(3) .0766(14) Uani d . 1 . C C4A .1834(3) .0322(3) 1.7111(4) .089(2) Uani d . 1 . C C5A .1459(4) -.0160(3) 1.6582(6) .111(2) Uani d . 1 . C C6A .1038(4) .0005(4) 1.5759(7) .115(2) Uani d . 1 . C C7A .0986(3) .0654(4) 1.5467(4) .099(2) Uani d . 1 . C C1B .3030(3) .0496(3) 1.4884(3) .0779(13) Uani d . 1 . C C2B .3855(2) .0614(2) 1.5259(3) .0617(11) Uani d . 1 . C C7B .4057(3) .0523(2) 1.6235(3) .0726(12) Uani d . 1 . C C6B .4801(4) .0693(3) 1.6592(4) .085(2) Uani d . 1 . C C5B .5382(3) .0964(3) 1.5994(5) .085(2) Uani d . 1 . C C4B .5215(3) .1058(3) 1.5031(4) .0838(14) Uani d . 1 . C C3B .4457(3) .0890(2) 1.4669(3) .0692(12) Uani d . 1 . C C1C .3390(3) .2176(2) 1.6090(4) .0817(14) Uani d . 1 . C C2C .3454(3) .2717(2) 1.5383(3) .0652(11) Uani d . 1 . C C7C .4096(3) .2747(3) 1.4722(4) .0774(13) Uani d . 1 . C C6C .4115(3) .3205(3) 1.3991(4) .089(2) Uani d . 1 . C C5C .3493(4) .3650(3) 1.3871(4) .106(2) Uani d . 1 . C C4C .2850(4) .3643(3) 1.4513(5) .096(2) Uani d . 1 . C C3C .2833(3) .3182(2) 1.5263(4) .0759(13) Uani d . 1 . C C1D .2746(3) .1814(3) 1.3429(3) .091(2) Uani d . 1 . C C2D .1880(3) .1766(3) 1.3169(3) .0668(12) Uani d . 1 . C C7D .1364(4) .2315(3) 1.3214(4) .086(2) Uani d . 1 . C C6D .0558(4) .2274(3) 1.3044(4) .096(2) Uani d . 1 . C C5D .0204(3) .1680(4) 1.2839(5) .099(2) Uani d . 1 . C C4D .0680(4) .1131(3) 1.2775(4) .099(2) Uani d . 1 . C C3D .1509(3) .1176(2) 1.2941(4) .0773(14) Uani d . 1 . C H1A .1434 .2189 1.6139 .119 Uiso d . 1 . H H2A .1020 .1974 1.5174 .119 Uiso d . 1 . H H7A .0684 .0756 1.4900 .134 Uiso d . 1 . H H6A .0785 -.0338 1.5393 .147 Uiso d . 1 . H H5A .1494 -.0614 1.6795 .138 Uiso d . 1 . H H4A .2121 .0203 1.7689 .107 Uiso d . 1 . H H3A .2085 .1306 1.7189 .098 Uiso d . 1 . H H1B .2717 .0202 1.5276 .097 Uiso d . 1 . H H2B .3026 .0341 1.4230 .097 Uiso d . 1 . H H7B .3659 .0342 1.6665 .087 Uiso d . 1 . H H6B .4922 .0617 1.7262 .104 Uiso d . 1 . H H5B .5900 .1087 1.6249 .105 Uiso d . 1 . H H4B .5619 .1240 1.4613 .103 Uiso d . 1 . H H3B .4345 .0965 1.3999 .086 Uiso d . 1 . H H1C .3106 .2294 1.6666 .099 Uiso d . 1 . H H2C .3901 .1981 1.6257 .099 Uiso d . 1 . H H7C .4533 .2439 1.4780 .095 Uiso d . 1 . H H6C .4571 .3214 1.3562 .108 Uiso d . 1 . H H5C .3510 .3958 1.3342 .128 Uiso d . 1 . H H4C .2418 .3950 1.4435 .119 Uiso d . 1 . H H3C .2385 .3190 1.5706 .093 Uiso d . 1 . H H1D .2955 .2249 1.3318 .118 Uiso d . 1 . H H2D .3066 .1496 1.3088 .118 Uiso d . 1 . H H7D .1590 .2738 1.3370 .108 Uiso d . 1 . H H6D .0237 .2672 1.3069 .118 Uiso d . 1 . H H5D -.0369 .1655 1.2735 .125 Uiso d . 1 . H H4D .0442 .0709 1.2619 .121 Uiso d . 1 . H H3D .1833 .0785 1.2894 .094 Uiso d . 1 . H 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_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C1C Zr1 C1B 115.0(2) yes C1C Zr1 C1D 118.8(2) yes C1B Zr1 C1D 95.7(2) yes C1C Zr1 C1A 95.8(2) yes C1B Zr1 C1A 121.3(2) yes C1D Zr1 C1A 112.0(2) yes C1C Zr1 C2A 105.3(2) yes C1B Zr1 C2A 88.9(2) yes C1D Zr1 C2A 128.0(2) yes C1A Zr1 C2A 33.3(2) yes C1C Zr1 C2C 32.93(15) yes C1B Zr1 C2C 134.17(15) yes C1D Zr1 C2C 87.8(2) yes C1A Zr1 C2C 98.8(2) yes C2A Zr1 C2C 123.9(2) yes C1C Zr1 C2B 85.0(2) yes C1B Zr1 C2B 31.84(14) yes C1D Zr1 C2B 102.2(2) yes C1A Zr1 C2B 140.0(2) yes C2A Zr1 C2B 107.96(15) yes C2C Zr1 C2B 102.76(14) yes C2A C1A Zr1 87.0(3) yes C3A C2A C7A 114.4(5) yes C3A C2A C1A 121.0(5) yes C7A C2A C1A 123.7(5) yes C3A C2A Zr1 95.1(3) yes C7A C2A Zr1 108.2(3) yes C1A C2A Zr1 59.7(2) yes C4A C3A C2A 122.8(5) yes C5A C4A C3A 120.1(6) yes C4A C5A C6A 120.2(6) yes C7A C6A C5A 120.4(6) yes C6A C7A C2A 122.0(6) yes C2B C1B Zr1 93.9(3) yes C7B C2B C3B 116.5(4) yes C7B C2B C1B 122.4(4) yes C3B C2B C1B 120.8(4) yes C7B C2B Zr1 111.7(3) yes C3B C2B Zr1 99.4(3) yes C1B C2B Zr1 54.2(2) yes C6B C7B C2B 121.9(5) yes C7B C6B C5B 120.4(5) yes C4B C5B C6B 119.8(5) yes C5B C4B C3B 119.9(5) yes C4B C3B C2B 121.6(5) yes C2C C1C Zr1 90.2(3) yes C7C C2C C3C 116.5(5) yes C7C C2C C1C 121.5(5) yes C3C C2C C1C 121.6(5) yes C7C C2C Zr1 106.8(3) yes C3C C2C Zr1 101.0(3) yes C1C C2C Zr1 56.9(2) yes C6C C7C C2C 122.0(5) yes C5C C6C C7C 120.8(5) yes C6C C5C C4C 119.2(5) yes C3C C4C C5C 120.1(5) yes C4C C3C C2C 121.4(5) yes C2D C1D Zr1 99.1(3) yes C3D C2D C7D 115.1(4) yes C3D C2D C1D 123.0(5) yes C7D C2D C1D 121.7(5) yes C6D C7D C2D 122.9(5) yes C7D C6D C5D 120.8(6) yes C6D C5D C4D 118.8(5) yes C5D C4D C3D 120.2(5) yes C2D C3D C4D 122.2(5) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Zr1 C1C 2.248(5) yes Zr1 C1B 2.255(5) yes Zr1 C1D 2.258(4) yes Zr1 C1A 2.259(5) yes Zr1 C2A 2.614(4) yes Zr1 C2C 2.684(4) yes Zr1 C2B 2.773(4) yes C1A C2A 1.437(7) yes C2A C3A 1.397(6) yes C2A C7A 1.428(8) yes C3A C4A 1.374(7) yes C4A C5A 1.355(8) yes C5A C6A 1.366(10) yes C6A C7A 1.363(9) yes C1B C2B 1.467(6) yes C2B C7B 1.395(6) yes C2B C3B 1.391(6) yes C7B C6B 1.358(7) yes C6B C5B 1.370(7) yes C5B C4B 1.366(7) yes C4B C3B 1.380(7) yes C1C C2C 1.459(6) yes C2C C7C 1.391(6) yes C2C C3C 1.390(6) yes C7C C6C 1.360(7) yes C6C C5C 1.364(8) yes C5C C4C 1.375(8) yes C4C C3C 1.383(8) yes C1D C2D 1.465(6) yes C2D C3D 1.365(6) yes C2D C7D 1.389(7) yes C7D C6D 1.344(7) yes C6D C5D 1.353(8) yes C5D C4D 1.352(8) yes C4D C3D 1.382(7) yes