#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2003028.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_2003028
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_sum            'C44 H60 Zr'
_chemical_formula_weight         680.14
_chemical_name_systematic        Tetrakis(p-ter-butylbenzyl)Zirconium
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.481(2)
_cell_length_b                   16.481(2)
_cell_length_c                   7.131(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      18
_cell_volume                     1936.9(11)
_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., 1990)'
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1512
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.47
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.311
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_description       prism
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.545
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.017
_refine_ls_goodness_of_fit_obs   1.053
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         1511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_restrained_S_obs      1.053
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_obs          0.033
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_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_wR_factor_all         0.0919
_refine_ls_wR_factor_obs         0.0822
_reflns_number_observed          1160
_reflns_number_total             1512
_reflns_observed_criterion       >2sigma(I)
_[local]_cod_data_source_file    na0084.cif
_[local]_cod_data_source_block   zrl
_[local]_cod_cif_authors_sg_H-M  I-4
_[local]_cod_chemical_formula_sum_orig 'C44 H60 Zr1'
_cod_original_cell_volume        1937.0(10)
_cod_database_code               2003028
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'
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 0.0522(2) 0.0522(2) 0.0356(2) 0.000 0.000 0.000
C1 0.052(2) 0.074(2) 0.049(2) -0.005(2) 0.000(2) 0.013(2)
C2 0.053(2) 0.052(2) 0.042(2) -0.0033(13) 0.0031(14) 0.0092(14)
C3 0.061(2) 0.056(2) 0.043(2) -0.0094(15) 0.0087(15) -0.0083(14)
C4 0.052(2) 0.049(2) 0.053(2) -0.0008(13) 0.010(2) -0.0103(15)
C5 0.053(2) 0.0464(15) 0.055(2) -0.0069(12) 0.0044(13) -0.0052(13)
C6 0.061(2) 0.0449(13) 0.061(2) -0.0040(11) 0.009(2) -0.013(2)
C7 0.058(2) 0.0488(14) 0.059(3) 0.0036(12) 0.013(2) -0.0020(14)
C8 0.0514(15) 0.060(2) 0.073(4) -0.0054(13) -0.006(2) -0.007(2)
C9 0.056(2) 0.118(4) 0.132(6) 0.007(2) -0.009(3) -0.041(4)
C10 0.083(3) 0.086(3) 0.080(3) -0.007(2) -0.016(3) 0.018(3)
C11 0.071(2) 0.080(2) 0.082(2) -0.028(2) -0.021(4) 0.015(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_type_symbol
Zr1 0.5000 0.0000 0.2500 0.0467(2) Uani d S 1 Zr
C1 0.5057(2) 0.1007(2) 0.0322(5) 0.0582(8) Uani d . 1 C
C2 0.5917(2) 0.1143(2) 0.0777(5) 0.0492(7) Uani d . 1 C
C3 0.6533(2) 0.0647(2) 0.0070(5) 0.0533(8) Uani d . 1 C
C4 0.7331(2) 0.0725(2) 0.0645(5) 0.0513(7) Uani d . 1 C
C5 0.7561(2) 0.1287(2) 0.2001(5) 0.0514(8) Uani d . 1 C
C6 0.6952(2) 0.1793(2) 0.2664(9) 0.0555(9) Uani d . 1 C
C7 0.6162(2) 0.1721(2) 0.2111(5) 0.0550(11) Uani d . 1 C
C8 0.8424(2) 0.1353(2) 0.2753(9) 0.0612(12) Uani d . 1 C
C9 0.9011(3) 0.0758(3) 0.1826(9) 0.102(2) Uani d . 1 C
C10 0.8415(3) 0.1161(3) 0.4885(8) 0.0832(13) Uani d . 1 C
C11 0.8751(2) 0.2215(2) 0.2498(12) 0.0775(10) Uani d . 1 C
H1 0.4950 0.0829 -0.0930 0.070 Uiso d . 1 H
H2 0.4707 0.1458 0.0590 0.070 Uiso d . 1 H
H3 0.6393 0.0229 -0.0820 0.065 Uiso d . 1 H
H4 0.7746 0.0397 0.0077 0.062 Uiso d . 1 H
H5 0.7093 0.2222 0.3471 0.069 Uiso d . 1 H
H6 0.5763 0.2066 0.2673 0.068 Uiso d . 1 H
H7 0.8823 0.0223 0.1944 0.123 Uiso d . 1 H
H8 0.9060 0.0892 0.0517 0.123 Uiso d . 1 H
H9 0.9536 0.0808 0.2384 0.123 Uiso d . 1 H
H10 0.8088 0.1542 0.5538 0.100 Uiso d . 1 H
H11 0.8217 0.0630 0.5099 0.100 Uiso d . 1 H
H12 0.8960 0.1195 0.5372 0.100 Uiso d . 1 H
H13 0.9284 0.2249 0.3039 0.091 Uiso d . 1 H
H14 0.8763 0.2359 0.1245 0.091 Uiso d . 1 H
H15 0.8409 0.2588 0.3190 0.091 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 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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_
_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
_geom_angle_publ_flag
C1 Zr1 C1 . 7 117.77(11) yes
C1 Zr1 C1 . 8_545 117.77(11) yes
C1 Zr1 C1 7 8_545 93.9(2) yes
C1 Zr1 C1 . 2_655 93.9(2) yes
C1 Zr1 C1 7 2_655 117.77(11) yes
C1 Zr1 C1 8_545 2_655 117.77(11) yes
C1 Zr1 C2 . . 32.88(11) yes
C1 Zr1 C2 7 . 86.06(12) yes
C1 Zr1 C2 8_545 . 133.44(11) yes
C1 Zr1 C2 2_655 . 102.77(12) yes
C1 Zr1 C2 . 7 133.44(11) yes
C1 Zr1 C2 7 7 32.88(11) yes
C1 Zr1 C2 8_545 7 102.77(12) yes
C1 Zr1 C2 2_655 7 86.06(12) yes
C2 Zr1 C2 . 7 101.86(6) yes
C1 Zr1 C2 . 8_545 86.06(12) yes
C1 Zr1 C2 7 8_545 102.77(12) yes
C1 Zr1 C2 8_545 8_545 32.88(11) yes
C1 Zr1 C2 2_655 8_545 133.44(11) yes
C2 Zr1 C2 . 8_545 101.86(6) yes
C2 Zr1 C2 7 8_545 126.08(15) yes
C1 Zr1 C2 . 2_655 102.77(12) yes
C1 Zr1 C2 7 2_655 133.44(11) yes
C1 Zr1 C2 8_545 2_655 86.06(12) yes
C1 Zr1 C2 2_655 2_655 32.88(11) yes
C2 Zr1 C2 . 2_655 126.08(15) yes
C2 Zr1 C2 7 2_655 101.86(6) yes
C2 Zr1 C2 8_545 2_655 101.86(6) yes
C2 C1 Zr1 . . 90.0(2) yes
C3 C2 C7 . . 115.6(3) yes
C3 C2 C1 . . 122.1(3) yes
C7 C2 C1 . . 121.9(3) yes
C3 C2 Zr1 . . 99.3(2) yes
C7 C2 Zr1 . . 108.9(2) yes
C1 C2 Zr1 . . 57.1(2) yes
C4 C3 C2 . . 122.0(3) yes
C3 C4 C5 . . 121.7(3) yes
C6 C5 C4 . . 116.1(3) yes
C6 C5 C8 . . 120.8(3) yes
C4 C5 C8 . . 123.1(3) yes
C7 C6 C5 . . 122.6(4) yes
C6 C7 C2 . . 121.8(3) yes
C5 C8 C11 . . 110.7(3) yes
C5 C8 C9 . . 113.1(4) yes
C11 C8 C9 . . 108.7(4) yes
C5 C8 C10 . . 108.8(4) yes
C11 C8 C10 . . 108.0(5) yes
C9 C8 C10 . . 107.4(4) yes
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
Zr1 C1 . 2.276(4) yes
Zr1 C1 7 2.276(4) yes
Zr1 C1 8_545 2.276(4) yes
Zr1 C1 2_655 2.276(4) yes
Zr1 C2 . 2.710(3) yes
Zr1 C2 7 2.710(3) yes
Zr1 C2 8_545 2.710(3) yes
Zr1 C2 2_655 2.710(3) yes
C1 C2 . 1.471(5) yes
C2 C3 . 1.397(5) yes
C2 C7 . 1.405(5) yes
C3 C4 . 1.385(5) yes
C4 C5 . 1.392(4) yes
C5 C6 . 1.387(5) yes
C5 C8 . 1.523(5) yes
C6 C7 . 1.367(5) yes
C8 C11 . 1.530(5) yes
C8 C9 . 1.528(6) yes
C8 C10 . 1.553(8) yes