#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:03:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179229 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/49/4314955.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_4314955
loop_
_publ_author_name
'Edmond Y. Njua'
'Alexander Steiner'
'Lothar Stahl'
_publ_contact_author_address
;Department of Chemistry
University of North Dakota
Grand Forks, ND 58202
USA
;
_publ_contact_author_email       lstahl@chem.und.edu
_publ_contact_author_fax         701-777-2331
_publ_contact_author_name        'Lothar Stahl'
_publ_contact_author_phone       701-777-2242
_publ_section_title
;
 Syntheses and Structures of Cationic and Neutral, Homo- and Heteroleptic
 tert-Butoxides of the Group 4 Metals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2163
_journal_page_last               2172
_journal_paper_doi               10.1021/ic9019537
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C24 H54 Hf O6 Sn'
_chemical_formula_weight         735.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           156
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2"'
_symmetry_space_group_name_H-M   'P 3 m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   17.0910(10)
_cell_length_b                   17.0910(10)
_cell_length_c                   9.4768(11)
_cell_measurement_temperature    173(2)
_cell_volume                     2397.3(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15175
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         4.13
_exptl_absorpt_coefficient_mu    4.056
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.45
_refine_diff_density_max         4.661
_refine_diff_density_min         -2.073
_refine_diff_density_rms         0.204
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         3061
_refine_ls_number_restraints     208
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0694
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+50.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1886
_refine_ls_wR_factor_ref         0.1902
_reflns_number_gt                2930
_reflns_number_total             3061
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9019537_si_001_1.cif
_cod_data_source_block           8
_cod_database_code               4314955
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Hf1 Hf 0.3333 -0.3333 0.67244(14) 0.0268(6) Uani 1 6 d SD . .
Sn1 Sn 0.3333 -0.3333 0.3372(5) 0.093(3) Uani 1 6 d SD . .
O1 O 0.3834(5) -0.3834(5) 0.4951(14) 0.053(6) Uiso 1 2 d SDU . .
C1 C 0.4306(6) -0.4306(6) 0.464(2) 0.056(10) Uiso 1 2 d SDU . .
C11 C 0.4574(9) -0.4574(9) 0.596(3) 0.067(10) Uiso 1 2 d SDU . .
H11A H 0.4973 -0.4044 0.6494 0.101 Uiso 0.50 1 calc PR . .
H11B H 0.4878 -0.4903 0.5738 0.101 Uiso 1 2 calc SR . .
H11C H 0.4046 -0.4950 0.6515 0.101 Uiso 0.50 1 calc PR . .
C12 C 0.375(2) -0.5107(19) 0.375(4) 0.150(18) Uiso 1 1 d DU . .
H12A H 0.3195 -0.5501 0.4232 0.225 Uiso 1 1 calc R . .
H12B H 0.4076 -0.5422 0.3582 0.225 Uiso 1 1 calc R . .
H12C H 0.3623 -0.4918 0.2873 0.225 Uiso 1 1 calc R . .
O2 O 0.2756(6) -0.4488(11) 0.7697(19) 0.056(7) Uiso 1 2 d SDU . .
C2 C 0.2364(7) -0.5272(13) 0.857(2) 0.046(8) Uiso 1 2 d SDU . .
C21 C 0.1948(10) -0.610(2) 0.770(5) 0.15(2) Uiso 1 2 d SDU . .
H21A H 0.2401 -0.6112 0.7112 0.218 Uiso 0.50 1 calc PR . .
H21B H 0.1482 -0.6116 0.7121 0.218 Uiso 0.50 1 calc PR . .
H21C H 0.1691 -0.6624 0.8307 0.218 Uiso 1 2 calc SR . .
C22 C 0.3072(18) -0.5311(19) 0.944(3) 0.096(10) Uiso 1 1 d DU . .
H22A H 0.3500 -0.5347 0.8825 0.144 Uiso 1 1 calc R . .
H22B H 0.2795 -0.5834 1.0034 0.144 Uiso 1 1 calc R . .
H22C H 0.3376 -0.4777 1.0008 0.144 Uiso 1 1 calc R . .
Hf2 Hf 0.0000 0.0000 -0.7794(4) 0.0257(4) Uani 1 6 d SD . .
Sn2 Sn 0.0000 0.0000 -0.4533(4) 0.090(2) Uani 1 6 d SD . .
O3 O -0.1011(11) -0.0506(5) -0.6108(18) 0.093(8) Uiso 1 2 d SDU . .
C3 C -0.1948(12) -0.0974(6) -0.574(2) 0.044(7) Uiso 1 2 d SDU . .
C31 C -0.254(2) -0.1272(11) -0.699(4) 0.12(2) Uiso 1 2 d SDU . .
H31A H -0.2514 -0.0756 -0.7445 0.182 Uiso 0.50 1 calc PR . .
H31B H -0.3154 -0.1680 -0.6703 0.182 Uiso 0.50 1 calc PR . .
H31C H -0.2349 -0.1573 -0.7636 0.182 Uiso 0.50 1 calc PR . .
C32 C -0.204(2) -0.0272(18) -0.495(3) 0.099(10) Uiso 1 1 d DU . .
H32A H -0.1685 -0.0113 -0.4107 0.148 Uiso 1 1 calc R . .
H32B H -0.2665 -0.0503 -0.4706 0.148 Uiso 1 1 calc R . .
H32C H -0.1839 0.0255 -0.5533 0.148 Uiso 1 1 calc R . .
O4 O -0.0561(7) 0.0561(7) -0.883(3) 0.115(10) Uiso 1 2 d SDU . .
C4 C -0.0987(7) 0.0987(7) -0.954(3) 0.064(10) Uiso 1 2 d SDU . .
C41 C -0.1323(10) 0.1323(10) -0.838(3) 0.078(11) Uiso 1 2 d SDU . .
H41A H -0.0820 0.1780 -0.7862 0.117 Uiso 0.50 1 calc PR . .
H41B H -0.1701 0.0832 -0.7767 0.117 Uiso 0.50 1 calc PR . .
H41C H -0.1667 0.1576 -0.8773 0.117 Uiso 0.50 1 calc PR . .
C42 C -0.165(2) 0.040(3) -1.059(4) 0.19(2) Uiso 1 1 d DU . .
H42A H -0.2128 -0.0123 -1.0124 0.291 Uiso 1 1 calc R . .
H42B H -0.1364 0.0204 -1.1264 0.291 Uiso 1 1 calc R . .
H42C H -0.1899 0.0719 -1.1065 0.291 Uiso 1 1 calc R . .
Hf3 Hf -0.3333 0.3333 -0.23205(19) 0.0322(7) Uani 1 6 d SD . .
Sn3 Sn -0.3333 0.3333 0.1032(3) 0.0348(11) Uani 1 6 d SD . .
O5 O -0.2332(10) 0.3834(5) -0.0529(16) 0.089(10) Uiso 1 2 d SDU . .
C5 C -0.1392(12) 0.4304(6) -0.024(2) 0.050(8) Uiso 1 2 d SDU . .
C51 C -0.084(2) 0.4578(11) -0.153(3) 0.102(17) Uiso 1 2 d SDU . .
H51A H -0.0918 0.5031 -0.2011 0.153 Uiso 0.50 1 calc PR . .
H51B H -0.1036 0.4063 -0.2133 0.153 Uiso 0.50 1 calc PR . .
H51C H -0.0219 0.4820 -0.1288 0.153 Uiso 0.50 1 calc PR . .
C52 C -0.110(3) 0.506(2) 0.074(4) 0.20(3) Uiso 1 1 d DU . .
H52A H -0.1221 0.5503 0.0345 0.304 Uiso 1 1 calc R . .
H52B H -0.0462 0.5326 0.0915 0.304 Uiso 1 1 calc R . .
H52C H -0.1421 0.4844 0.1619 0.304 Uiso 1 1 calc R . .
O6 O -0.2769(5) 0.4463(10) -0.3282(18) 0.051(6) Uiso 1 2 d SDU . .
C6 C -0.2387(7) 0.5225(14) -0.421(3) 0.056(9) Uiso 1 2 d SDU . .
C61 C -0.1981(9) 0.6038(19) -0.328(4) 0.12(2) Uiso 1 2 d SDU . .
H61A H -0.2452 0.6069 -0.2774 0.182 Uiso 0.50 1 calc PR . .
H61B H -0.1652 0.6571 -0.3842 0.182 Uiso 0.50 1 calc PR . .
H61C H -0.1578 0.5995 -0.2618 0.182 Uiso 0.50 1 calc PR . .
C62 C -0.1686(18) 0.522(2) -0.515(3) 0.102(11) Uiso 1 1 d DU . .
H62A H -0.1961 0.4696 -0.5742 0.153 Uiso 1 1 calc R . .
H62B H -0.1222 0.5219 -0.4589 0.153 Uiso 1 1 calc R . .
H62C H -0.1427 0.5755 -0.5734 0.153 Uiso 1 1 calc R . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Hf1 O2 99.3(8) 3_655 2_545 ?
O2 Hf1 O2 99.3(8) 3_655 . ?
O2 Hf1 O2 99.3(8) 2_545 . ?
O2 Hf1 O1 93.7(5) 3_655 3_655 ?
O2 Hf1 O1 159.8(7) 2_545 3_655 ?
O2 Hf1 O1 93.7(5) . 3_655 ?
O2 Hf1 O1 93.7(5) 3_655 2_545 ?
O2 Hf1 O1 93.7(5) 2_545 2_545 ?
O2 Hf1 O1 159.8(7) . 2_545 ?
O1 Hf1 O1 69.9(6) 3_655 2_545 ?
O2 Hf1 O1 159.8(7) 3_655 . ?
O2 Hf1 O1 93.7(5) 2_545 . ?
O2 Hf1 O1 93.7(5) . . ?
O1 Hf1 O1 69.9(6) 3_655 . ?
O1 Hf1 O1 69.9(6) 2_545 . ?
O2 Hf1 Sn1 118.3(6) 3_655 . ?
O2 Hf1 Sn1 118.3(6) 2_545 . ?
O2 Hf1 Sn1 118.3(6) . . ?
O1 Hf1 Sn1 41.4(4) 3_655 . ?
O1 Hf1 Sn1 41.4(4) 2_545 . ?
O1 Hf1 Sn1 41.4(4) . . ?
O1 Sn1 O1 75.1(6) 2_545 3_655 ?
O1 Sn1 O1 75.1(6) 2_545 . ?
O1 Sn1 O1 75.1(6) 3_655 . ?
O1 Sn1 Hf1 44.8(4) 2_545 . ?
O1 Sn1 Hf1 44.8(4) 3_655 . ?
O1 Sn1 Hf1 44.8(4) . . ?
C1 O1 Sn1 122.9(11) . . ?
C1 O1 Hf1 143.2(12) . . ?
Sn1 O1 Hf1 93.8(6) . . ?
O1 C1 C12 110.9(15) . . ?
O1 C1 C12 110.9(15) . 4 ?
C12 C1 C12 103(3) . 4 ?
O1 C1 C11 110.5(16) . . ?
C12 C1 C11 110.5(16) . . ?
C12 C1 C11 110.5(16) 4 . ?
C2 O2 Hf1 172.8(16) . . ?
O2 C2 C21 110.6(19) . . ?
O2 C2 C22 110.6(13) . . ?
C21 C2 C22 105.9(15) . . ?
O2 C2 C22 110.6(13) . 5_655 ?
C21 C2 C22 105.9(15) . 5_655 ?
C22 C2 C22 113(3) . 5_655 ?
O4 Hf2 O4 96.3(11) 2 . ?
O4 Hf2 O4 96.3(11) 2 3 ?
O4 Hf2 O4 96.3(11) . 3 ?
O4 Hf2 O3 163.8(10) 2 3 ?
O4 Hf2 O3 94.5(7) . 3 ?
O4 Hf2 O3 94.5(7) 3 3 ?
O4 Hf2 O3 94.5(7) 2 . ?
O4 Hf2 O3 94.5(7) . . ?
O4 Hf2 O3 163.8(10) 3 . ?
O3 Hf2 O3 72.6(7) 3 . ?
O4 Hf2 O3 94.5(7) 2 2 ?
O4 Hf2 O3 163.8(10) . 2 ?
O4 Hf2 O3 94.5(7) 3 2 ?
O3 Hf2 O3 72.6(7) 3 2 ?
O3 Hf2 O3 72.6(7) . 2 ?
O4 Hf2 Sn2 120.6(8) 2 . ?
O4 Hf2 Sn2 120.6(8) . . ?
O4 Hf2 Sn2 120.6(8) 3 . ?
O3 Hf2 Sn2 43.1(4) 3 . ?
O3 Hf2 Sn2 43.1(4) . . ?
O3 Hf2 Sn2 43.1(4) 2 . ?
O3 Sn2 O3 75.7(7) . 3 ?
O3 Sn2 O3 75.7(7) . 2 ?
O3 Sn2 O3 75.7(7) 3 2 ?
O3 Sn2 Hf2 45.1(4) . . ?
O3 Sn2 Hf2 45.1(4) 3 . ?
O3 Sn2 Hf2 45.1(4) 2 . ?
C3 O3 Sn2 120.9(12) . . ?
C3 O3 Hf2 147.3(13) . . ?
Sn2 O3 Hf2 91.8(6) . . ?
O3 C3 C31 112.3(18) . . ?
O3 C3 C32 102.4(13) . . ?
C31 C3 C32 110.2(13) . . ?
O3 C3 C32 102.4(13) . 6 ?
C31 C3 C32 110.2(13) . 6 ?
C32 C3 C32 119(3) . 6 ?
C4 O4 Hf2 177(2) . . ?
O4 C4 C42 112.6(17) . . ?
O4 C4 C42 112.6(17) . 4 ?
C42 C4 C42 94(4) . 4 ?
O4 C4 C41 104.1(17) . . ?
C42 C4 C41 116.8(18) . . ?
C42 C4 C41 116.8(18) 4 . ?
O6 Hf3 O6 99.0(7) 3_455 2_565 ?
O6 Hf3 O6 99.0(7) 3_455 . ?
O6 Hf3 O6 99.0(7) 2_565 . ?
O6 Hf3 O5 94.1(5) 3_455 . ?
O6 Hf3 O5 159.7(7) 2_565 . ?
O6 Hf3 O5 94.1(5) . . ?
O6 Hf3 O5 94.1(5) 3_455 3_455 ?
O6 Hf3 O5 94.1(5) 2_565 3_455 ?
O6 Hf3 O5 159.7(7) . 3_455 ?
O5 Hf3 O5 69.4(6) . 3_455 ?
O6 Hf3 O5 159.7(7) 3_455 2_565 ?
O6 Hf3 O5 94.1(5) 2_565 2_565 ?
O6 Hf3 O5 94.1(5) . 2_565 ?
O5 Hf3 O5 69.4(6) . 2_565 ?
O5 Hf3 O5 69.4(6) 3_455 2_565 ?
O6 Hf3 Sn3 118.6(6) 3_455 . ?
O6 Hf3 Sn3 118.6(6) 2_565 . ?
O6 Hf3 Sn3 118.6(6) . . ?
O5 Hf3 Sn3 41.1(4) . . ?
O5 Hf3 Sn3 41.1(4) 3_455 . ?
O5 Hf3 Sn3 41.1(4) 2_565 . ?
O5 Sn3 O5 75.6(6) 3_455 . ?
O5 Sn3 O5 75.6(6) 3_455 2_565 ?
O5 Sn3 O5 75.6(6) . 2_565 ?
O5 Sn3 Hf3 45.1(4) 3_455 . ?
O5 Sn3 Hf3 45.1(4) . . ?
O5 Sn3 Hf3 45.1(4) 2_565 . ?
C5 O5 Sn3 123.8(12) . . ?
C5 O5 Hf3 142.4(13) . . ?
Sn3 O5 Hf3 93.8(6) . . ?
O5 C5 C52 114.6(17) . 6_565 ?
O5 C5 C52 114.6(17) . . ?
C52 C5 C52 91(4) 6_565 . ?
O5 C5 C51 112.2(18) . . ?
C52 C5 C51 111.5(18) 6_565 . ?
C52 C5 C51 111.5(18) . . ?
C6 O6 Hf3 170.7(16) . . ?
O6 C6 C61 105.8(17) . . ?
O6 C6 C62 111.5(14) . 5_455 ?
C61 C6 C62 110.8(15) . 5_455 ?
O6 C6 C62 111.5(14) . . ?
C61 C6 C62 110.8(15) . . ?
C62 C6 C62 107(3) 5_455 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hf1 O2 1.941(13) 3_655 ?
Hf1 O2 1.941(13) 2_545 ?
Hf1 O2 1.941(13) . ?
Hf1 O1 2.242(13) 3_655 ?
Hf1 O1 2.242(13) 2_545 ?
Hf1 O1 2.242(13) . ?
Hf1 Sn1 3.177(5) . ?
Sn1 O1 2.107(14) 2_545 ?
Sn1 O1 2.107(14) 3_655 ?
Sn1 O1 2.107(14) . ?
O1 C1 1.427(17) . ?
C1 C12 1.477(17) . ?
C1 C12 1.477(17) 4 ?
C1 C11 1.482(17) . ?
O2 C2 1.426(16) . ?
C2 C21 1.483(18) . ?
C2 C22 1.489(16) . ?
C2 C22 1.489(16) 5_655 ?
Hf2 O4 1.929(16) 2 ?
Hf2 O4 1.929(16) . ?
Hf2 O4 1.929(16) 3 ?
Hf2 O3 2.190(16) 3 ?
Hf2 O3 2.190(16) . ?
Hf2 O3 2.190(16) 2 ?
Hf2 Sn2 3.090(4) . ?
Sn2 O3 2.113(17) . ?
Sn2 O3 2.113(17) 3 ?
Sn2 O3 2.113(17) 2 ?
O3 C3 1.430(17) . ?
C3 C31 1.479(18) . ?
C3 C32 1.489(16) . ?
C3 C32 1.489(16) 6 ?
O4 C4 1.431(17) . ?
C4 C42 1.465(17) . ?
C4 C42 1.465(17) 4 ?
C4 C41 1.483(17) . ?
Hf3 O6 1.904(13) 3_455 ?
Hf3 O6 1.904(13) 2_565 ?
Hf3 O6 1.904(13) . ?
Hf3 O5 2.254(15) . ?
Hf3 O5 2.254(15) 3_455 ?
Hf3 O5 2.254(15) 2_565 ?
Hf3 Sn3 3.177(3) . ?
Sn3 O5 2.094(16) 3_455 ?
Sn3 O5 2.094(16) . ?
Sn3 O5 2.094(16) 2_565 ?
O5 C5 1.419(17) . ?
C5 C52 1.461(17) 6_565 ?
C5 C52 1.461(17) . ?
C5 C51 1.470(17) . ?
O6 C6 1.431(17) . ?
C6 C61 1.492(18) . ?
C6 C62 1.496(16) 5_455 ?
C6 C62 1.496(16) . ?
