#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:03:56 +0100 (Wed, 23 Mar 2016) $
#$Revision: 179229 $
#$URL: svn://saulius.grazulis.lt/cod-secondary/cif/4/31/49/4314956.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_4314956
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 H51 Cl3 O6 Sn Zr'
_chemical_formula_weight         751.91
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           146
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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                   14.7142(9)
_cell_length_b                   14.7142(9)
_cell_length_c                   13.8699(16)
_cell_measurement_reflns_used    6703
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.06
_cell_measurement_theta_min      2.77
_cell_volume                     2600.6(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.906
_diffrn_measured_fraction_theta_max 0.906
_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  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5383
_diffrn_reflns_theta_full        28.17
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    1.282
_exptl_absorpt_correction_T_max  0.7483
_exptl_absorpt_correction_T_min  0.4715
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_coef       0.00184(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2368
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0227
_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/[\s^2^(Fo^2^)+(0.0166P)^2^+1.2157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0589
_reflns_number_gt                2356
_reflns_number_total             2368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9019537_si_001_2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4314956
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
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
Zr1 Zr 1.0000 0.0000 0.664556(18) 0.02930(9) Uani 1 3 d S . .
Sn1 Sn 0.3333 0.6667 0.81663(2) 0.07767(16) Uani 1 3 d S . .
Cl1 Cl 0.47534(7) 0.66801(8) 0.91196(7) 0.0732(2) Uani 1 1 d . . .
O1 O 0.87102(12) -0.10119(12) 0.72512(13) 0.0402(3) Uani 1 1 d . . .
O2 O 1.12867(11) 0.09724(11) 0.55071(12) 0.0356(3) Uani 1 1 d . B .
C1 C 0.7773(2) -0.15069(19) 0.7818(2) 0.0454(6) Uani 1 1 d . . .
C2 C 0.7494(3) -0.2637(2) 0.7991(3) 0.0782(11) Uani 1 1 d . . .
H2A H 0.7309 -0.3018 0.7377 0.117 Uiso 1 1 calc R . .
H2B H 0.6896 -0.2973 0.8434 0.117 Uiso 1 1 calc R . .
H2C H 0.8098 -0.2651 0.8275 0.117 Uiso 1 1 calc R . .
C3 C 0.7984(3) -0.0901(3) 0.8741(3) 0.0850(11) Uani 1 1 d . . .
H3A H 0.8611 -0.0839 0.9051 0.128 Uiso 1 1 calc R . .
H3B H 0.7381 -0.1269 0.9174 0.128 Uiso 1 1 calc R . .
H3C H 0.8097 -0.0199 0.8601 0.128 Uiso 1 1 calc R . .
C4 C 0.6907(2) -0.1481(3) 0.7250(3) 0.0633(8) Uani 1 1 d . . .
H4A H 0.7114 -0.0751 0.7099 0.095 Uiso 1 1 calc R . .
H4B H 0.6261 -0.1797 0.7634 0.095 Uiso 1 1 calc R . .
H4C H 0.6785 -0.1876 0.6649 0.095 Uiso 1 1 calc R . .
C5 C 1.23831(19) 0.1275(2) 0.5642(2) 0.0569(7) Uani 1 1 d D . .
H5A H 1.2455 0.0660 0.5808 0.068 Uiso 1 1 calc R A 1
H5B H 1.2709 0.1808 0.6158 0.068 Uiso 1 1 calc R A 1
C6A C 1.2881(3) 0.1730(3) 0.4662(3) 0.0576(13) Uiso 0.669(10) 1 d PDU B 1
H6A1 H 1.3640 0.2242 0.4729 0.069 Uiso 0.669(10) 1 calc PR B 1
H6A2 H 1.2787 0.1169 0.4210 0.069 Uiso 0.669(10) 1 calc PR B 1
C6B C 1.2992(6) 0.2339(7) 0.5122(7) 0.057(3) Uiso 0.331(10) 1 d PDU B 2
H6B1 H 1.3116 0.2924 0.5556 0.068 Uiso 0.331(10) 1 calc PR B 2
H6B2 H 1.3674 0.2455 0.4878 0.068 Uiso 0.331(10) 1 calc PR B 2
C8 C 1.12180(19) 0.1581(2) 0.4717(2) 0.0515(6) Uani 1 1 d . . .
H8A H 1.0936 0.2028 0.4947 0.062 Uiso 1 1 calc R B .
H8B H 1.0749 0.1110 0.4206 0.062 Uiso 1 1 calc R . .
C7 C 1.2306(2) 0.2244(3) 0.4336(3) 0.0773(10) Uani 1 1 d D B .
H7A H 1.2301 0.2276 0.3623 0.093 Uiso 1 1 calc R C 1
H7B H 1.2628 0.2967 0.4595 0.093 Uiso 1 1 calc R C 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zr1 0.02964(10) 0.02964(10) 0.0286(2) 0.000 0.000 0.01482(5)
Sn1 0.0979(2) 0.0979(2) 0.0372(3) 0.000 0.000 0.04896(10)
Cl1 0.0655(5) 0.0875(5) 0.0733(6) 0.0119(4) 0.0246(4) 0.0432(4)
O1 0.0345(7) 0.0396(8) 0.0417(10) 0.0038(7) 0.0087(6) 0.0150(6)
O2 0.0320(7) 0.0378(7) 0.0362(9) 0.0042(7) 0.0013(6) 0.0169(6)
C1 0.0411(11) 0.0437(12) 0.0474(14) 0.0103(10) 0.0165(10) 0.0183(10)
C2 0.0719(19) 0.0563(16) 0.108(3) 0.0407(18) 0.043(2) 0.0336(14)
C3 0.074(2) 0.102(3) 0.053(2) -0.0068(18) 0.0236(16) 0.0247(19)
C4 0.0451(14) 0.0736(18) 0.073(2) 0.0143(16) 0.0115(13) 0.0311(13)
C5 0.0306(11) 0.0668(17) 0.0635(18) 0.0165(14) 0.0048(10) 0.0169(11)
C8 0.0467(13) 0.0548(14) 0.0525(15) 0.0230(11) 0.0077(11) 0.0251(11)
C7 0.0500(15) 0.0718(19) 0.088(3) 0.0389(18) 0.0112(15) 0.0140(13)
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 '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'
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
O1 Zr1 O1 102.35(6) 3_765 . ?
O1 Zr1 O1 102.35(6) 3_765 2_645 ?
O1 Zr1 O1 102.35(6) . 2_645 ?
O1 Zr1 O2 87.06(6) 3_765 2_645 ?
O1 Zr1 O2 89.05(7) . 2_645 ?
O1 Zr1 O2 163.11(6) 2_645 2_645 ?
O1 Zr1 O2 163.11(6) 3_765 3_765 ?
O1 Zr1 O2 87.06(6) . 3_765 ?
O1 Zr1 O2 89.05(7) 2_645 3_765 ?
O2 Zr1 O2 79.02(6) 2_645 3_765 ?
O1 Zr1 O2 89.05(7) 3_765 . ?
O1 Zr1 O2 163.11(6) . . ?
O1 Zr1 O2 87.06(6) 2_645 . ?
O2 Zr1 O2 79.02(6) 2_645 . ?
O2 Zr1 O2 79.02(6) 3_765 . ?
Cl1 Sn1 Cl1 93.91(3) 2_665 3_565 ?
Cl1 Sn1 Cl1 93.91(3) 2_665 . ?
Cl1 Sn1 Cl1 93.91(3) 3_565 . ?
C1 O1 Zr1 164.00(15) . . ?
C8 O2 C5 108.48(18) . . ?
C8 O2 Zr1 127.29(12) . . ?
C5 O2 Zr1 122.52(15) . . ?
O1 C1 C3 107.8(2) . . ?
O1 C1 C4 108.0(2) . . ?
C3 C1 C4 110.8(3) . . ?
O1 C1 C2 108.0(2) . . ?
C3 C1 C2 112.2(3) . . ?
C4 C1 C2 109.9(3) . . ?
O2 C5 C6A 103.6(3) . . ?
O2 C5 C6B 104.1(4) . . ?
C6A C5 C6B 39.7(4) . . ?
C7 C6A C5 103.1(3) . . ?
C7 C6B C5 103.5(5) . . ?
O2 C8 C7 106.7(2) . . ?
C6B C7 C6A 42.1(4) . . ?
C6B C7 C8 105.3(4) . . ?
C6A C7 C8 105.1(3) . . ?
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
Zr1 O1 1.9232(15) 3_765 ?
Zr1 O1 1.9232(15) . ?
Zr1 O1 1.9232(15) 2_645 ?
Zr1 O2 2.3272(15) 2_645 ?
Zr1 O2 2.3272(15) 3_765 ?
Zr1 O2 2.3272(15) . ?
Sn1 Cl1 2.4644(10) 2_665 ?
Sn1 Cl1 2.4644(10) 3_565 ?
Sn1 Cl1 2.4644(10) . ?
O1 C1 1.430(3) . ?
O2 C8 1.450(3) . ?
O2 C5 1.455(3) . ?
C1 C3 1.501(5) . ?
C1 C4 1.516(4) . ?
C1 C2 1.520(4) . ?
C5 C6A 1.531(5) . ?
C5 C6B 1.540(9) . ?
C6A C7 1.461(5) . ?
C6B C7 1.444(9) . ?
C8 C7 1.494(4) . ?
